# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_boran
_database_code_depnum_ccdc_archive 'CCDC 2034385'
loop_
_audit_author_name
_audit_author_address
'Florian Kleemiss'
;University of Bern
Switzerland
;
_audit_update_record             
;
2020-09-28 deposited with the CCDC.	2020-11-09 downloaded from the CCDC.
;
_audit_creation_date             2020-03-10
_audit_creation_method           
;
Olex2 1.3-dev
(compiled 2020.01.16 svn.ra754ea2f for OlexSys, GUI svn.r6014)
;
_chemical_formula_moiety         '4.001(H2 N0.5), 0.5(B12 H12)'
_chemical_formula_sum            'B6.001 H14.002 N2'
_chemical_formula_weight         107.087
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_dispersion_source
H 0.00000 0.00000 Sasaki
B 0.00000 0.00000 Sasaki
N 0.00000 0.00000 Sasaki

_space_group_crystal_system      cubic
_space_group_IT_number           225
_space_group_name_H-M_alt        'F m -3 m'
_space_group_name_Hall           '-F 4 2 3'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 x,-z,y
3 x,z,-y
4 z,y,-x
5 -z,y,x
6 -y,x,z
7 y,-x,z
8 z,x,y
9 y,z,x
10 -y,-z,x
11 z,-x,-y
12 -y,z,-x
13 -z,-x,y
14 -z,x,-y
15 y,-z,-x
16 x,-y,-z
17 -x,y,-z
18 -x,-y,z
19 y,x,-z
20 -y,-x,-z
21 z,-y,x
22 -z,-y,-x
23 -x,z,y
24 -x,-z,-y
25 -x,-y,-z
26 -x,z,-y
27 -x,-z,y
28 -z,-y,x
29 z,-y,-x
30 y,-x,-z
31 -y,x,-z
32 -z,-x,-y
33 -y,-z,-x
34 y,z,-x
35 -z,x,y
36 y,-z,x
37 z,x,-y
38 z,-x,y
39 -y,z,x
40 -x,y,z
41 x,-y,z
42 x,y,-z
43 -y,-x,z
44 y,x,z
45 -z,y,-x
46 z,y,x
47 x,-z,-y
48 x,z,y
49 x,y+1/2,z+1/2
50 x,-z+1/2,y+1/2
51 x,z+1/2,-y+1/2
52 z,y+1/2,-x+1/2
53 -z,y+1/2,x+1/2
54 -y,x+1/2,z+1/2
55 y,-x+1/2,z+1/2
56 z,x+1/2,y+1/2
57 y,z+1/2,x+1/2
58 -y,-z+1/2,x+1/2
59 z,-x+1/2,-y+1/2
60 -y,z+1/2,-x+1/2
61 -z,-x+1/2,y+1/2
62 -z,x+1/2,-y+1/2
63 y,-z+1/2,-x+1/2
64 x,-y+1/2,-z+1/2
65 -x,y+1/2,-z+1/2
66 -x,-y+1/2,z+1/2
67 y,x+1/2,-z+1/2
68 -y,-x+1/2,-z+1/2
69 z,-y+1/2,x+1/2
70 -z,-y+1/2,-x+1/2
71 -x,z+1/2,y+1/2
72 -x,-z+1/2,-y+1/2
73 -x,-y+1/2,-z+1/2
74 -x,z+1/2,-y+1/2
75 -x,-z+1/2,y+1/2
76 -z,-y+1/2,x+1/2
77 z,-y+1/2,-x+1/2
78 y,-x+1/2,-z+1/2
79 -y,x+1/2,-z+1/2
80 -z,-x+1/2,-y+1/2
81 -y,-z+1/2,-x+1/2
82 y,z+1/2,-x+1/2
83 -z,x+1/2,y+1/2
84 y,-z+1/2,x+1/2
85 z,x+1/2,-y+1/2
86 z,-x+1/2,y+1/2
87 -y,z+1/2,x+1/2
88 -x,y+1/2,z+1/2
89 x,-y+1/2,z+1/2
90 x,y+1/2,-z+1/2
91 -y,-x+1/2,z+1/2
92 y,x+1/2,z+1/2
93 -z,y+1/2,-x+1/2
94 z,y+1/2,x+1/2
95 x,-z+1/2,-y+1/2
96 x,z+1/2,y+1/2
97 x+1/2,y,z+1/2
98 x+1/2,-z,y+1/2
99 x+1/2,z,-y+1/2
100 z+1/2,y,-x+1/2
101 -z+1/2,y,x+1/2
102 -y+1/2,x,z+1/2
103 y+1/2,-x,z+1/2
104 z+1/2,x,y+1/2
105 y+1/2,z,x+1/2
106 -y+1/2,-z,x+1/2
107 z+1/2,-x,-y+1/2
108 -y+1/2,z,-x+1/2
109 -z+1/2,-x,y+1/2
110 -z+1/2,x,-y+1/2
111 y+1/2,-z,-x+1/2
112 x+1/2,-y,-z+1/2
113 -x+1/2,y,-z+1/2
114 -x+1/2,-y,z+1/2
115 y+1/2,x,-z+1/2
116 -y+1/2,-x,-z+1/2
117 z+1/2,-y,x+1/2
118 -z+1/2,-y,-x+1/2
119 -x+1/2,z,y+1/2
120 -x+1/2,-z,-y+1/2
121 -x+1/2,-y,-z+1/2
122 -x+1/2,z,-y+1/2
123 -x+1/2,-z,y+1/2
124 -z+1/2,-y,x+1/2
125 z+1/2,-y,-x+1/2
126 y+1/2,-x,-z+1/2
127 -y+1/2,x,-z+1/2
128 -z+1/2,-x,-y+1/2
129 -y+1/2,-z,-x+1/2
130 y+1/2,z,-x+1/2
131 -z+1/2,x,y+1/2
132 y+1/2,-z,x+1/2
133 z+1/2,x,-y+1/2
134 z+1/2,-x,y+1/2
135 -y+1/2,z,x+1/2
136 -x+1/2,y,z+1/2
137 x+1/2,-y,z+1/2
138 x+1/2,y,-z+1/2
139 -y+1/2,-x,z+1/2
140 y+1/2,x,z+1/2
141 -z+1/2,y,-x+1/2
142 z+1/2,y,x+1/2
143 x+1/2,-z,-y+1/2
144 x+1/2,z,y+1/2
145 x+1/2,y+1/2,z
146 x+1/2,-z+1/2,y
147 x+1/2,z+1/2,-y
148 z+1/2,y+1/2,-x
149 -z+1/2,y+1/2,x
150 -y+1/2,x+1/2,z
151 y+1/2,-x+1/2,z
152 z+1/2,x+1/2,y
153 y+1/2,z+1/2,x
154 -y+1/2,-z+1/2,x
155 z+1/2,-x+1/2,-y
156 -y+1/2,z+1/2,-x
157 -z+1/2,-x+1/2,y
158 -z+1/2,x+1/2,-y
159 y+1/2,-z+1/2,-x
160 x+1/2,-y+1/2,-z
161 -x+1/2,y+1/2,-z
162 -x+1/2,-y+1/2,z
163 y+1/2,x+1/2,-z
164 -y+1/2,-x+1/2,-z
165 z+1/2,-y+1/2,x
166 -z+1/2,-y+1/2,-x
167 -x+1/2,z+1/2,y
168 -x+1/2,-z+1/2,-y
169 -x+1/2,-y+1/2,-z
170 -x+1/2,z+1/2,-y
171 -x+1/2,-z+1/2,y
172 -z+1/2,-y+1/2,x
173 z+1/2,-y+1/2,-x
174 y+1/2,-x+1/2,-z
175 -y+1/2,x+1/2,-z
176 -z+1/2,-x+1/2,-y
177 -y+1/2,-z+1/2,-x
178 y+1/2,z+1/2,-x
179 -z+1/2,x+1/2,y
180 y+1/2,-z+1/2,x
181 z+1/2,x+1/2,-y
182 z+1/2,-x+1/2,y
183 -y+1/2,z+1/2,x
184 -x+1/2,y+1/2,z
185 x+1/2,-y+1/2,z
186 x+1/2,y+1/2,-z
187 -y+1/2,-x+1/2,z
188 y+1/2,x+1/2,z
189 -z+1/2,y+1/2,-x
190 z+1/2,y+1/2,x
191 x+1/2,-z+1/2,-y
192 x+1/2,z+1/2,y

_symmetry_Int_Tables_number      225
_cell_length_a                   9.10295(12)
_cell_length_b                   9.10295(12)
_cell_length_c                   9.10295(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     754.304(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    100.00(10)
_cell_measurement_reflns_used    2677
_cell_measurement_theta_min      3.8490
_cell_measurement_theta_max      75.7830
_cell_oxdiff_length_a            9.1026(3)
_cell_oxdiff_length_b            9.1026(2)
_cell_oxdiff_length_c            9.1036(3)
_cell_oxdiff_angle_alpha         90.021(3)
_cell_oxdiff_angle_beta          89.981(3)
_cell_oxdiff_angle_gamma         89.996(3)
_cell_oxdiff_volume              754.30(4)
_cell_oxdiff_measurement_reflns_used 2677
_exptl_absorpt_correction_T_min  0.71007
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.38b (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.917
_oxdiff_exptl_absorpt_empirical_full_max 1.207
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_exptl_absorpt_coefficient_mu    0.046
_exptl_crystal_density_diffrn    0.943
_exptl_crystal_F_000             232.0
_diffrn_reflns_av_R_equivalents  0.0243
_diffrn_reflns_av_unetI/netI     0.0117
_diffrn_reflns_Laue_measured_fraction_full 1.0000
_diffrn_reflns_Laue_measured_fraction_max 1.0000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            4841
_diffrn_reflns_point_group_measured_fraction_full 1.0000
_diffrn_reflns_point_group_measured_fraction_max 1.0000
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         62.47
_diffrn_reflns_theta_min         3.88
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 1.0000
_diffrn_measured_fraction_theta_max 1.0000
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              13
_reflns_limit_h_min              0
_reflns_limit_k_max              22
_reflns_limit_k_min              1
_reflns_limit_l_max              16
_reflns_limit_l_min              0
_reflns_number_gt                341
_reflns_number_total             364
_reflns_threshold_expression     I>=2u(I)
_computing_molecular_graphics    'Olex2 1.3-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.3-dev (Bourhis et al., 2015)'
_refine_diff_density_max         0.1093
_refine_diff_density_min         -0.0662
_refine_diff_density_rms         0.0131
_refine_ls_d_res_high            0.4007
_refine_ls_d_res_low             5.2556
_refine_ls_goodness_of_fit_ref   0.9106
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     11
_refine_ls_number_reflns         364
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0105
_refine_ls_R_factor_gt           0.0095
_refine_ls_restrained_S_all      1.0180
_refine_ls_shift/su_max          0.0002
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0110P)²+0.0085P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0234
_refine_ls_wR_factor_ref         0.0236
_diffrn_ambient_environment      N~2~
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, Pilatus 300K'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Pilatus 300K'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0332405000
_diffrn_orient_matrix_UB_12      0.0675561000
_diffrn_orient_matrix_UB_13      -0.0200556000
_diffrn_orient_matrix_UB_21      0.0529070000
_diffrn_orient_matrix_UB_22      -0.0092625000
_diffrn_orient_matrix_UB_23      0.0564269000
_diffrn_orient_matrix_UB_31      0.0465604000
_diffrn_orient_matrix_UB_32      -0.0377135000
_diffrn_orient_matrix_UB_33      -0.0498435000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -5.00  73.00   0.25   20.00    --    0.00  19.00-180.00  312
  2  ω     19.00  77.00   0.25   55.00    --   84.25 -83.00 -68.00  232
  3  ω    -49.00   8.00   0.25   20.00    --    0.00   0.00-180.00  228
  4  ω    -74.00 -32.00   0.25   55.00    -- -105.75  19.00-120.00  168
  5  ω    -74.00 -32.00   0.25   55.00    -- -105.75  19.00 -90.00  168
  6  ω   -178.00-100.00   0.25   55.00    -- -105.75 -19.00   0.00  312
;
_refine_special_details          
;
Refinement using NoSpherA2, an implementation of
 NOn-SPHERical Atom-form-factors in Olex2.
Please cite:
F. Kleemiss, H. Puschmann, O. Dolomanov, S.Grabowsky - to be published - 2020
NoSpherA2 implementation of HAR makes use of
 tailor-made aspherical atomic form factors calculated
on-the-fly from a Hirshfeld-partitioned electron density (ED) - not from
spherical-atom form factors.

The ED is calculated from a gaussian basis set single determinant SCF
wavefunction - either Hartree-Fock or DFT using selected funtionals
 - for a fragment of the crystal.
This fregment can be embedded in an electrostatic crystal field by employing cluster charges.
The following options were used:
   SOFTWARE:       ORCA
   PARTITIONING:   NoSpherA2
   INT ACCURACY:   High
   METHOD:         PBE
   BASIS SET:      def2-TZVPP
   CHARGE:         6
   MULTIPLICITY:   1
   DATE:           2020-06-19_12-42-38
;

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
N1 N 0.25 0.25 0.25 0.01112(2) Uani 1.000080 24 S T P
B1 B 0.365268(13) 0.5 0.5 0.01009(2) Uani 1.000000 8 S T P
H1 H 0.2332(4) 0.5 0.5 0.0292(9) Uani 1.000000 8 S T P
H1a H 0.3146(2) 0.1854(2) 0.1854(2) 0.0351(9) Uani 1.000020 6 S T P


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 H1a 1.019(3) . ?
N1 H1a 1.019(3) 64 ?
N1 H1a 1.019(3) 8 ?
N1 H1a 1.019(3) 9 ?
B1 B1 1.73447(16) 4_556 ?
B1 B1 1.73447(16) 6_655 ?
B1 B1 1.73447(16) 7_565 ?
B1 B1 1.73447(16) 5_655 ?
B1 H1 1.203(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
H1a N1 H1a 109.5 8 . ?
H1a N1 H1a 109.5 64 8 ?
H1a N1 H1a 109.47(11) 64 . ?
H1a N1 H1a 109.5 9 . ?
H1a N1 H1a 109.5 9 8 ?
H1a N1 H1a 109.5 64 9 ?
B1 B1 B1 60.0 6_655 5_655 ?
B1 B1 B1 60.0 7_565 5_655 ?
B1 B1 B1 90.0 7_565 6_655 ?
H1 B1 B1 135.0 . 5_655 ?
H1 B1 B1 135.0 . 7_565 ?
H1 B1 B1 135.0 . 6_655 ?

# start Validation Reply Form
_vrf_PLAT303_boran               
;
PROBLEM: Full Occupancy Atom H1A       with # Connections       9.00 Check 
RESPONSE: Due to the high symmetry and correct bondlengths compared to spherical density descirption of X-ray data the authors are confident the geometry is correct
;
_vrf_PLAT927_boran               
;
PROBLEM: Reported and Calculated  wR2 Differ by .........    -0.0877 Check 
RESPONSE: Non-Spherical refinement, therefore wR2 from CheckCIF is wrong
;
_vrf_PLAT928_boran               
;
PROBLEM: Reported and Calculated    S value   Differ by .     -3.586 Check 
RESPONSE: Non-Spherical refinement, therefore S from CheckCIF is wrong
;
_vrf_PLAT049_boran               
;
PROBLEM: Calculated Density Less Than 1.0 gcm-3 .........     0.9422 Check 
RESPONSE: This structure consists of many light atoms
;
_vrf_PLAT926_boran               
;
PROBLEM: Reported and Calculated   R1 Differ by .........    -0.0247 Check 
RESPONSE: Non-Spherical refinement, therefore R1 from CheckCIF is wrong
;
# end Validation Reply Form


_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_CaF2
_database_code_depnum_ccdc_archive 'CCDC 2034386'
loop_
_audit_author_name
_audit_author_address
'Florian Kleemiss'
;University of Bern
Switzerland
;
_audit_update_record             
;
2020-09-28 deposited with the CCDC.	2020-11-09 downloaded from the CCDC.
;
_audit_creation_date             2020-03-13
_audit_creation_method           
;
Olex2 1.3-dev
(compiled 2020.03.04 svn.rc2590c38 for OlexSys, GUI svn.r6014)
;
_chemical_formula_moiety         'Ca1 F2'
_chemical_formula_sum            'Ca F2'
_chemical_formula_weight         78.075
_chemical_oxdiff_formula         'Ca F'
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_dispersion_source
Ca 0.13779 0.19369 Sasaki
F 0.00604 0.00613 Sasaki

_vrf_PLAT974_CaF2                
;
PROBLEM: Check Calcd Negative Resid. Density on      Ca01      -2.41 eA-3  
RESPONSE: Residual densities calculated by CheckCIF are based on spherical densities
;
_vrf_PLAT112_CaF2                
;
PROBLEM: ADDSYM Detects New (Pseudo) Symm. Elem         4        100 %Fit  
RESPONSE: The high symmetry in SG number 225 contains all recommended symmetry elements
;
_vrf_PLAT927_CaF2                
;
PROBLEM: Reported and Calculated  wR2 Differ by .........    -0.0241 Check 
RESPONSE: Statistics calculated by CheckCIF cannot account for non-spherical refinements
;
_vrf_PLAT928_CaF2                
;
PROBLEM: Reported and Calculated    S value   Differ by .     -0.949 Check 
RESPONSE: Statistics calculated by CheckCIF cannot account for non-spherical refinements
;

_space_group_crystal_system      cubic
_space_group_IT_number           225
_space_group_name_H-M_alt        'F m -3 m'
_space_group_name_Hall           '-F 4 2 3'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 x,-z,y
3 x,z,-y
4 z,y,-x
5 -z,y,x
6 -y,x,z
7 y,-x,z
8 z,x,y
9 y,z,x
10 -y,-z,x
11 z,-x,-y
12 -y,z,-x
13 -z,-x,y
14 -z,x,-y
15 y,-z,-x
16 x,-y,-z
17 -x,y,-z
18 -x,-y,z
19 y,x,-z
20 -y,-x,-z
21 z,-y,x
22 -z,-y,-x
23 -x,z,y
24 -x,-z,-y
25 -x,-y,-z
26 -x,z,-y
27 -x,-z,y
28 -z,-y,x
29 z,-y,-x
30 y,-x,-z
31 -y,x,-z
32 -z,-x,-y
33 -y,-z,-x
34 y,z,-x
35 -z,x,y
36 y,-z,x
37 z,x,-y
38 z,-x,y
39 -y,z,x
40 -x,y,z
41 x,-y,z
42 x,y,-z
43 -y,-x,z
44 y,x,z
45 -z,y,-x
46 z,y,x
47 x,-z,-y
48 x,z,y
49 x,y+1/2,z+1/2
50 x,-z+1/2,y+1/2
51 x,z+1/2,-y+1/2
52 z,y+1/2,-x+1/2
53 -z,y+1/2,x+1/2
54 -y,x+1/2,z+1/2
55 y,-x+1/2,z+1/2
56 z,x+1/2,y+1/2
57 y,z+1/2,x+1/2
58 -y,-z+1/2,x+1/2
59 z,-x+1/2,-y+1/2
60 -y,z+1/2,-x+1/2
61 -z,-x+1/2,y+1/2
62 -z,x+1/2,-y+1/2
63 y,-z+1/2,-x+1/2
64 x,-y+1/2,-z+1/2
65 -x,y+1/2,-z+1/2
66 -x,-y+1/2,z+1/2
67 y,x+1/2,-z+1/2
68 -y,-x+1/2,-z+1/2
69 z,-y+1/2,x+1/2
70 -z,-y+1/2,-x+1/2
71 -x,z+1/2,y+1/2
72 -x,-z+1/2,-y+1/2
73 -x,-y+1/2,-z+1/2
74 -x,z+1/2,-y+1/2
75 -x,-z+1/2,y+1/2
76 -z,-y+1/2,x+1/2
77 z,-y+1/2,-x+1/2
78 y,-x+1/2,-z+1/2
79 -y,x+1/2,-z+1/2
80 -z,-x+1/2,-y+1/2
81 -y,-z+1/2,-x+1/2
82 y,z+1/2,-x+1/2
83 -z,x+1/2,y+1/2
84 y,-z+1/2,x+1/2
85 z,x+1/2,-y+1/2
86 z,-x+1/2,y+1/2
87 -y,z+1/2,x+1/2
88 -x,y+1/2,z+1/2
89 x,-y+1/2,z+1/2
90 x,y+1/2,-z+1/2
91 -y,-x+1/2,z+1/2
92 y,x+1/2,z+1/2
93 -z,y+1/2,-x+1/2
94 z,y+1/2,x+1/2
95 x,-z+1/2,-y+1/2
96 x,z+1/2,y+1/2
97 x+1/2,y,z+1/2
98 x+1/2,-z,y+1/2
99 x+1/2,z,-y+1/2
100 z+1/2,y,-x+1/2
101 -z+1/2,y,x+1/2
102 -y+1/2,x,z+1/2
103 y+1/2,-x,z+1/2
104 z+1/2,x,y+1/2
105 y+1/2,z,x+1/2
106 -y+1/2,-z,x+1/2
107 z+1/2,-x,-y+1/2
108 -y+1/2,z,-x+1/2
109 -z+1/2,-x,y+1/2
110 -z+1/2,x,-y+1/2
111 y+1/2,-z,-x+1/2
112 x+1/2,-y,-z+1/2
113 -x+1/2,y,-z+1/2
114 -x+1/2,-y,z+1/2
115 y+1/2,x,-z+1/2
116 -y+1/2,-x,-z+1/2
117 z+1/2,-y,x+1/2
118 -z+1/2,-y,-x+1/2
119 -x+1/2,z,y+1/2
120 -x+1/2,-z,-y+1/2
121 -x+1/2,-y,-z+1/2
122 -x+1/2,z,-y+1/2
123 -x+1/2,-z,y+1/2
124 -z+1/2,-y,x+1/2
125 z+1/2,-y,-x+1/2
126 y+1/2,-x,-z+1/2
127 -y+1/2,x,-z+1/2
128 -z+1/2,-x,-y+1/2
129 -y+1/2,-z,-x+1/2
130 y+1/2,z,-x+1/2
131 -z+1/2,x,y+1/2
132 y+1/2,-z,x+1/2
133 z+1/2,x,-y+1/2
134 z+1/2,-x,y+1/2
135 -y+1/2,z,x+1/2
136 -x+1/2,y,z+1/2
137 x+1/2,-y,z+1/2
138 x+1/2,y,-z+1/2
139 -y+1/2,-x,z+1/2
140 y+1/2,x,z+1/2
141 -z+1/2,y,-x+1/2
142 z+1/2,y,x+1/2
143 x+1/2,-z,-y+1/2
144 x+1/2,z,y+1/2
145 x+1/2,y+1/2,z
146 x+1/2,-z+1/2,y
147 x+1/2,z+1/2,-y
148 z+1/2,y+1/2,-x
149 -z+1/2,y+1/2,x
150 -y+1/2,x+1/2,z
151 y+1/2,-x+1/2,z
152 z+1/2,x+1/2,y
153 y+1/2,z+1/2,x
154 -y+1/2,-z+1/2,x
155 z+1/2,-x+1/2,-y
156 -y+1/2,z+1/2,-x
157 -z+1/2,-x+1/2,y
158 -z+1/2,x+1/2,-y
159 y+1/2,-z+1/2,-x
160 x+1/2,-y+1/2,-z
161 -x+1/2,y+1/2,-z
162 -x+1/2,-y+1/2,z
163 y+1/2,x+1/2,-z
164 -y+1/2,-x+1/2,-z
165 z+1/2,-y+1/2,x
166 -z+1/2,-y+1/2,-x
167 -x+1/2,z+1/2,y
168 -x+1/2,-z+1/2,-y
169 -x+1/2,-y+1/2,-z
170 -x+1/2,z+1/2,-y
171 -x+1/2,-z+1/2,y
172 -z+1/2,-y+1/2,x
173 z+1/2,-y+1/2,-x
174 y+1/2,-x+1/2,-z
175 -y+1/2,x+1/2,-z
176 -z+1/2,-x+1/2,-y
177 -y+1/2,-z+1/2,-x
178 y+1/2,z+1/2,-x
179 -z+1/2,x+1/2,y
180 y+1/2,-z+1/2,x
181 z+1/2,x+1/2,-y
182 z+1/2,-x+1/2,y
183 -y+1/2,z+1/2,x
184 -x+1/2,y+1/2,z
185 x+1/2,-y+1/2,z
186 x+1/2,y+1/2,-z
187 -y+1/2,-x+1/2,z
188 y+1/2,x+1/2,z
189 -z+1/2,y+1/2,-x
190 z+1/2,y+1/2,x
191 x+1/2,-z+1/2,-y
192 x+1/2,z+1/2,y

_symmetry_Int_Tables_number      225
_cell_length_a                   5.45095(5)
_cell_length_b                   5.45095(5)
_cell_length_c                   5.45095(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     161.963(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6248
_cell_measurement_temperature    100.0(10)
_cell_measurement_theta_max      65.6870
_cell_measurement_theta_min      5.0900
_exptl_crystal_description       block
_exptl_absorpt_coefficient_mu    1.747
_exptl_absorpt_correction_T_max  0.895
_exptl_absorpt_correction_T_min  0.776
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    3.202
_exptl_crystal_F_000             152.597
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
2 -1 1 0.1314
0 -1 0 0.1160
-1 -2 2 0.0676
1 0 1 0.1219
1 0 2 0.1147
0 2 1 0.1446
1 2 -1 0.0891
1 2 2 0.1164
0 0 -1 0.1362
2 1 2 0.1044
-2 1 -2 0.0900
-1 -2 -2 0.1498
1 1 -1 0.0643
-1 1 -1 0.0693
1 2 -2 0.0676
0 0 1 0.0947
-2 -1 2 0.0573
1 -2 -1 0.1285
1 -2 0 0.1096
1 -2 1 0.1020
-2 1 -1 0.0731
-1 -2 1 0.0617
1 1 1 0.0946
-2 -1 1 0.0470
-1 2 -2 0.0640
-1 -1 1 0.0403
2 1 -1 0.0576
1 1 2 0.0989

_exptl_crystal_size_max          0.304
_exptl_crystal_size_mid          0.205
_exptl_crystal_size_min          0.105
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
1.9980 -0.9956 1.0082 0.2453 0.0521 -0.0151
0.0005 -0.9990 0.0055 0.0382 0.0457 0.0833
-1.0010 -1.9945 2.0089 0.0276 0.2969 0.0768
0.9981 0.0027 1.0013 0.1145 0.0449 -0.0771
0.9969 0.0048 2.0010 0.1364 0.1283 -0.1327
-0.0022 2.0001 0.9889 -0.0546 -0.0080 -0.2224
0.9998 1.9966 -1.0092 -0.0057 -0.2134 -0.1324
0.9960 2.0028 1.9901 0.0599 0.0369 -0.2994
0.0013 -0.0021 -0.9998 -0.0219 -0.0834 0.0557
1.9958 1.0044 1.9971 0.1908 0.0440 -0.2375
-1.9967 0.9935 -2.0080 -0.2672 -0.1355 0.0708
-0.9960 -2.0028 -1.9901 -0.0599 -0.0369 0.2994
1.0002 0.9976 -1.0037 0.0325 -0.1677 -0.0491
-0.9986 0.9963 -1.0067 -0.1527 -0.0906 -0.0063
1.0010 1.9945 -2.0089 -0.0276 -0.2969 -0.0768
-0.0013 0.0021 0.9998 0.0219 0.0834 -0.0557
-2.0009 -0.9962 2.0020 -0.1032 0.2897 0.0148
1.0016 -1.9994 -0.9874 0.1472 -0.0305 0.2010
1.0003 -1.9973 0.0124 0.1691 0.0529 0.1453
0.9990 -1.9953 1.0122 0.1910 0.1363 0.0896
-1.9980 0.9956 -1.0082 -0.2453 -0.0521 0.0151
-0.9998 -1.9966 1.0092 0.0057 0.2134 0.1324
0.9977 1.0017 0.9958 0.0763 -0.0008 -0.1604
-1.9996 -0.9982 1.0022 -0.1251 0.2063 0.0705
-0.9978 1.9932 -2.0119 -0.2128 -0.2198 -0.0340
-1.0002 -0.9976 1.0037 -0.0325 0.1677 0.0491
1.9996 0.9982 -1.0022 0.1251 -0.2063 -0.0705
0.9964 1.0038 1.9956 0.0981 0.0826 -0.2161

_diffrn_reflns_av_R_equivalents  0.0673
_diffrn_reflns_av_unetI/netI     0.0117
_diffrn_reflns_Laue_measured_fraction_full 1.0000
_diffrn_reflns_Laue_measured_fraction_max 1.0000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5299
_diffrn_reflns_point_group_measured_fraction_full 1.0000
_diffrn_reflns_point_group_measured_fraction_max 1.0000
_diffrn_reflns_theta_full        19.6651
_diffrn_reflns_theta_max         44.26
_diffrn_reflns_theta_min         5.11
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.97(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.0000
_diffrn_measured_fraction_theta_max 1.0000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -18.00  73.00   1.00    5.00    --    0.00  65.00-147.00   91
  2  ω     74.00 149.00   1.00   20.00    --   86.25  47.00 -55.00   75
  3  ω     82.00 149.00   1.00   20.00    --   86.25 110.00  24.00   67
  4  ω     74.00 149.00   1.00   20.00    --   86.25  19.00 150.00   75
  5  ω     74.00 149.00   1.00   20.00    --   86.25  19.00  30.00   75
  6  ω     72.00 149.00   1.00   20.00    --   86.25  57.00-120.00   77
  7  ω     74.00 149.00   1.00   20.00    --   86.25  37.00-150.00   75
  8  ω     72.00 149.00   1.00   20.00    --   86.25  57.00 -30.00   77
  9  ω     72.00 149.00   1.00   20.00    --   86.25  57.00  60.00   77
 10  ω     72.00 149.00   1.00   20.00    --   86.25  57.00 150.00   77
 11  ω     14.00  53.00   1.00   20.00    --   86.25 -65.00  76.00   39
 12  ω     14.00  81.00   1.00   20.00    --   86.25 -99.00   0.00   67
 13  ω     14.00  81.00   1.00   20.00    --   86.25 -77.00  12.00   67
 14  ω     14.00  41.00   1.00   20.00    --   86.25 -57.00 150.00   27
 15  ω     14.00 115.00   1.00   20.00    --   86.25 -88.00 136.03  101
 16  ω     14.00  41.00   1.00   20.00    --   86.25 -57.00 -90.00   27
 17  ω     14.00  41.00   1.00   20.00    --   86.25 -57.00-150.00   27
 18  ω     14.00  41.00   1.00   20.00    --   86.25 -57.00-180.00   27
 19  ω     14.00 114.00   1.00   20.00    --   86.25 -87.00-107.96  100
 20  ω    -12.00  76.00   1.00    5.00    --    0.00  19.00 150.00   88
 21  ω    -12.00  60.00   1.00    5.00    --    0.00  19.00  90.00   72
 22  ω    -22.00  34.00   1.00    5.00    --    0.00 -99.00  60.00   56
 23  ω    -22.00  34.00   1.00    5.00    --    0.00 -99.00 120.00   56
 24  ω    -42.00 -12.00   1.00   20.00    --  -40.25 -88.00 160.39   30
 25  ω    -41.00 -10.00   1.00   20.00    --  -40.25 -92.00  78.08   31
 26  ω    -75.00 -50.00   1.00   40.00    --  -40.25 110.00  24.00   25
 27  ω     91.00 116.00   1.00   40.00    --   86.25 110.00  24.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0926552000
_diffrn_orient_matrix_UB_12      -0.0381070000
_diffrn_orient_matrix_UB_13      0.0220841000
_diffrn_orient_matrix_UB_21      -0.0386687000
_diffrn_orient_matrix_UB_22      -0.0453312000
_diffrn_orient_matrix_UB_23      0.0834962000
_diffrn_orient_matrix_UB_31      -0.0212714000
_diffrn_orient_matrix_UB_32      -0.0837436000
_diffrn_orient_matrix_UB_33      -0.0555333000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Ag K\a'
_diffrn_radiation_wavelength     0.56087
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Ag) X-ray Source'
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              7
_reflns_limit_h_min              0
_reflns_limit_k_max              13
_reflns_limit_k_min              1
_reflns_limit_l_max              9
_reflns_limit_l_min              0
_reflns_number_gt                96
_reflns_number_total             96
_reflns_odcompleteness_completeness 95.02
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     44.37
_reflns_threshold_expression     I>=2u(I)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.3-dev (Bourhis et al., 2015)'
_refine_diff_density_max         0.6860
_refine_diff_density_min         -0.4146
_refine_diff_density_rms         0.0898
_refine_ls_d_res_high            0.4018
_refine_ls_d_res_low             3.1471
_refine_ls_goodness_of_fit_ref   1.0864
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     3
_refine_ls_number_reflns         96
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0114
_refine_ls_R_factor_gt           0.0114
_refine_ls_restrained_S_all      1.0864
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0175P)²+0.0607P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0279
_refine_ls_wR_factor_ref         0.0279
_refine_special_details          
;
Refinement using NoSpherA2, an implementation of
 NOn-SPHERical Atom-form-factors in Olex2.
Please cite:
F. Kleemiss, H. Puschmann, O. Dolomanov, S.Grabowsky - to be published - 2020
NoSpherA2 implementation of HAR makes use of
 tailor-made aspherical atomic form factors calculated
on-the-fly from a Hirshfeld-partitioned electron density (ED) - not from
spherical-atom form factors.

The ED is calculated from a gaussian basis set single determinant SCF
wavefunction - either Hartree-Fock or DFT using selected funtionals
 - for a fragment of the crystal.
This fregment can be embedded in an electrostatic crystal field by employing cluster charges.
The following options were used:
   SOFTWARE:       ORCA
   PARTITIONING:   NoSpherA2
   INT ACCURACY:   High
   METHOD:         PBE
   BASIS SET:      def2-TZVPP
   CHARGE:         18
   MULTIPLICITY:   1
   DATE:           2020-06-17_15-21-20
;
_olex2_refinement_description    
;
;

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Ca01 Ca 0.5 0.5 0.5 0.00334(4) Uani 0.999840 48 S T P
F002 F 0.25 0.75 0.75 0.00505(6) Uani 1.000080 24 S T P


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ca01 Ca01 3.85440(3) 49_554 ?
Ca01 F002 2.360331(12) 1_555 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
F002 Ca01 Ca01 144.7356(3) 49_544 97 ?
F002 Ca01 Ca01 35.2644(3) 57_545 97 ?
F002 Ca01 F002 70.5288(6) 56_554 52_545 ?
F002 Ca01 F002 109.4712(6) 57_545 56_554 ?
Ca01 F002 Ca01 109.4712(6) 59_566 11_566 ?


_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.970
_oxdiff_exptl_absorpt_empirical_full_min 0.709
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_L-Ala_23K_NoSpherA2_ORCA_NoSpherA2
_database_code_depnum_ccdc_archive 'CCDC 2035147'
loop_
_audit_author_name
_audit_author_address
'Florian Kleemiss'
;University of Bern
Switzerland
;
_audit_update_record             
;
2020-10-02 deposited with the CCDC.	2020-11-09 downloaded from the CCDC.
;

_audit_creation_date             2020-17-11
_audit_creation_method           
;
Olex2 1.3-dev
(compiled 2020.01.16 svn.ra754ea2f for OlexSys, GUI svn.r6014)
;

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_moiety         'C3 H7 N O2'
_chemical_formula_sum            'C3 H7 N O2'
_chemical_formula_weight         89.0947
_chemical_absolute_configuration syn

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'p 21 21 21'
_symmetry_space_group_name_Hall  'p 2ac 2ab'
_symmetry_Int_Tables_number      19
loop_
_symmetry_equiv_pos_as_xyz
'+x, +y, +z'
'-x+1/2, -y, +z+1/2'
'+x+1/2, -y+1/2, -z'
'-x, +y+1/2, -z+1/2'

_cell_length_a                   5.9279(10)
_cell_length_b                   12.2597(17)
_cell_length_c                   5.7939(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     421.07(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    23
_cell_measurement_wavelength     0.71073
_cell_measurement_theta_min      15.00
_cell_measurement_theta_max      22.50
_cell_measurement_reflns_used    1524

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       sphere
_exptl_crystal_colour            colorless
_exptl_crystal_size_rad          0.18
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             192

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.117
_exptl_absorpt_correction_type   none

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      23
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_probe          x-ray
_diffrn_measurement_method       'area detector'
_diffrn_measurement_device_type  'P-1 four circle diffractometer'
_diffrn_standards_number         0
_diffrn_reflns_av_unetI/netI     0.0243
_diffrn_reflns_number            2387
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         50.14
_diffrn_reflns_theta_min         3.32
_diffrn_measured_fraction_theta_full 0.9641
_diffrn_measured_fraction_theta_max 0.9412
_diffrn_reflns_point_group_measured_fraction_full 0.9641
_diffrn_reflns_point_group_measured_fraction_max 0.9412
_reflns_Friedel_fraction_full    0
_reflns_Friedel_fraction_max     0
_reflns_Friedel_coverage         0.0
_reflns_number_gt                2387
_reflns_number_total             2387
_reflns_threshold_expression     I/u(I)>2.1

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2008)'
_computing_structure_refinement  'olex2.refine 1.3-dev (Bourhis et al., 2015)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_hydrogens   difmap

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
_atom_type_scat_dispersion_source
H 0.00000 0.00000 'NoSPherA2 (see refine special details)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
C 0.00347 0.00161 'NoSPherA2 (see refine special details)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
O 0.01158 0.00611 'NoSPherA2 (see refine special details)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
N 0.00653 0.00323 'NoSPherA2 (see refine special details)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'

_refine_diff_density_max         0.1628
_refine_diff_density_min         -0.1652
_refine_diff_density_rms         0.0419
_refine_ls_d_res_high            0.4630
_refine_ls_d_res_low             6.1299
_refine_ls_goodness_of_fit_ref   1.2147
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     118
_refine_ls_number_reflns         2387
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0196
_refine_ls_R_factor_gt           0.0196
_refine_ls_restrained_S_all      1.2147
_refine_ls_shift/su_max          0.0005
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     w=1/[σ²(Fo²)]
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0332
_refine_ls_wR_factor_ref         0.0332
_refine_special_details          
;
Refinement using NoSpherA2, an implementation of 
NOn-SPHERical Atom-form-factors in Olex2.
Please cite:

F. Kleemiss, H. Puschmann, O. Dolomanov, S.Grabowsky - to be publsihed - 2020
NoSpherA2 makes use of tailor-made aspherical atomic form factors calculated
on-the-fly from a Hirshfeld-partitioned electron density (ED) - not from
spherical-atom form factors.

The ED is calculated from a gaussian basis set single determinant SCF
wavefunction - either Hartree-Fock or B3LYP 
- for a fragment of the crystal embedded in
an electrostatic crystal field.
The following options were used:
   SOFTWARE:       ORCA
   METHOD:         rhf
   BASIS SET:      6-311G(d,p)
   CHARGE:         0
   MULTIPLICITY:   1
   DATE:           2020-01-29_13-41-33
;

#----------------------------------------------------------------------------#
#                    VALIDATION REPLY FORM                                   #
#----------------------------------------------------------------------------#

_vrf_PLAT881_L-Ala_23K_NoSpherA2_ORCA_NoSpherA2 
;
PROBLEM: No Datum for _diffrn_reflns_av_R_equivalents ...     Please Do !  
RESPONSE: The dataset used corresponds to the CCDC number 1203202 (CSD code 
LALNIN03), which is merged. No information on Rmerge was provided by the
previous authors. 
;
_vrf_PLAT926_L-Ala_23K_NoSpherA2_ORCA_NoSpherA2 
;
PROBLEM: Reported and Calculated   R1 Differ by .........    -0.0111 Check 
RESPONSE: Because CheckCIF is unable to treat aspherical refinements.
;
_vrf_PLAT927_L-Ala_23K_NoSpherA2_ORCA_NoSpherA2 
;
PROBLEM: Reported and Calculated  wR2 Differ by .........    -0.0452 Check 
RESPONSE: Because CheckCIF is unable to treat aspherical refinements.
;
_vrf_PLAT928_L-Ala_23K_NoSpherA2_ORCA_NoSpherA2 
;
PROBLEM: Reported and Calculated    S value   Differ by .     -1.657 Check 
RESPONSE: Because CheckCIF is unable to treat aspherical refinements.
;

# end Validation Reply Form
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_refinement_flags_posn
N1 N 0.64723(5) 0.13752(2) 0.18292(5) 0.00536(4) Uani 1.000000 .
H1a H 0.7039(13) 0.0593(6) 0.2015(15) 0.026(2) Uani 1.000000 .
H1b H 0.7774(12) 0.1900(5) 0.2116(15) 0.0230(19) Uani 1.000000 .
H1c H 0.5805(12) 0.1495(5) 0.0182(14) 0.0239(19) Uani 1.000000 .
C1 C 0.46639(5) 0.16112(2) 0.35429(5) 0.00464(4) Uani 1.000000 .
H1 H 0.4267(10) 0.2481(4) 0.3426(12) 0.0218(17) Uani 1.000000 .
C2 C 0.25992(5) 0.09066(3) 0.30333(6) 0.00710(4) Uani 1.000000 .
H2a H 0.1911(11) 0.1102(5) 0.1333(13) 0.030(2) Uani 1.000000 .
H2b H 0.1259(12) 0.1046(6) 0.4304(14) 0.030(2) Uani 1.000000 .
H2c H 0.3031(10) 0.0052(5) 0.3083(14) 0.030(2) Uani 1.000000 .
C3 C 0.55406(5) 0.14079(2) 0.59985(5) 0.00440(4) Uani 1.000000 .
O1 O 0.72667(4) 0.083801(18) 0.62429(4) 0.00651(4) Uani 1.000000 .
O2 O 0.44091(4) 0.184009(18) 0.76109(4) 0.00632(3) Uani 1.000000 .


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 H1a 1.022(7) . ?
N1 H1b 1.018(7) . ?
N1 H1c 1.044(8) . ?
N1 C1 1.4895(4) . ?
C1 H1 1.094(5) . ?
C1 C2 1.5269(4) . ?
C1 C3 1.5351(5) . ?
C2 H2a 1.093(7) . ?
C2 H2b 1.096(7) . ?
C2 H2c 1.079(6) . ?
C3 O1 1.2471(4) . ?
C3 O2 1.2662(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
H1b N1 H1a 109.1(5) . . ?
H1c N1 H1a 110.7(6) . . ?
H1c N1 H1b 110.3(6) . . ?
C1 N1 H1a 110.4(5) . . ?
C1 N1 H1b 108.3(4) . . ?
C1 N1 H1c 108.0(4) . . ?
H1 C1 N1 107.6(3) . . ?
C2 C1 N1 109.76(3) . . ?
C2 C1 H1 111.5(3) . . ?
C3 C1 N1 110.04(2) . . ?
C3 C1 H1 106.8(4) . . ?
C3 C1 C2 111.02(2) . . ?
H2a C2 C1 110.5(3) . . ?
H2b C2 C1 111.3(4) . . ?
H2b C2 H2a 107.5(5) . . ?
H2c C2 C1 110.7(3) . . ?
H2c C2 H2a 109.0(5) . . ?
H2c C2 H2b 107.8(5) . . ?
O1 C3 C1 118.30(3) . . ?
O2 C3 C1 115.88(3) . . ?
O2 C3 O1 125.82(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C3 O1 -18.15(3) . . . . ?
N1 C1 C3 O2 162.19(2) . . . . ?


# END of CIF
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Pau100m71
_database_code_depnum_ccdc_archive 'CCDC 2034389'
loop_
_audit_author_name
_audit_author_address
'Florian Kleemiss'
;University of Bern
Switzerland
;
_audit_update_record             
;
2020-09-28 deposited with the CCDC.	2020-11-09 downloaded from the CCDC.
;
_audit_creation_date             2020-06-19
_audit_creation_method           
;
Olex2 1.3-dev
(compiled 2020.04.27 svn.r7e0b91c7 for OlexSys, GUI svn.r6014)
;
_chemical_formula_moiety         'C6 H6 O2, C0.286 O0.57'
_chemical_formula_sum            'C6.286 H6 O2.57'
_chemical_formula_weight         122.681
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_dispersion_source
H 0.00000 0.00000 Sasaki
C 0.00210 0.00160 Sasaki
O 0.00790 0.00610 Sasaki

_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3'
_space_group_name_Hall           '-R 3'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -y,x-y,z
3 -x+y,-x,z
4 -x,-y,-z
5 y,-x+y,-z
6 x-y,x,-z
7 x+1/3,y+2/3,z+2/3
8 -y+1/3,x-y+2/3,z+2/3
9 -x+y+1/3,-x+2/3,z+2/3
10 -x+1/3,-y+2/3,-z+2/3
11 y+1/3,-x+y+2/3,-z+2/3
12 x-y+1/3,x+2/3,-z+2/3
13 x+2/3,y+1/3,z+1/3
14 -y+2/3,x-y+1/3,z+1/3
15 -x+y+2/3,-x+1/3,z+1/3
16 -x+2/3,-y+1/3,-z+1/3
17 y+2/3,-x+y+1/3,-z+1/3
18 x-y+2/3,x+1/3,-z+1/3

_symmetry_Int_Tables_number      148
_cell_length_a                   16.2023(11)
_cell_length_b                   16.2023(11)
_cell_length_c                   5.6943(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1294.57(15)
_cell_formula_units_Z            9
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    7311
_cell_measurement_theta_min      2.51
_cell_measurement_theta_max      37.99

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_exptl_absorpt_coefficient_mu    0.111
_exptl_absorpt_correction_type   multi-scans
_exptl_absorpt_correction_T_min  0.7063
_exptl_absorpt_correction_T_max  0.7475
_exptl_absorpt_process_details   'SADABS (Bruker-AXS)'
_exptl_crystal_density_diffrn    1.416
_exptl_crystal_F_000             578.780

_diffrn_reflns_av_R_equivalents  0.0173
_diffrn_reflns_av_unetI/netI     0.0133
_diffrn_reflns_Laue_measured_fraction_full 0.9527
_diffrn_reflns_Laue_measured_fraction_max 0.9408
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            8426
_diffrn_reflns_point_group_measured_fraction_full 0.9527
_diffrn_reflns_point_group_measured_fraction_max 0.9408
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         37.99
_diffrn_reflns_theta_min         3.86
_diffrn_measured_fraction_theta_full 0.9527
_diffrn_measured_fraction_theta_max 0.9408
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              23
_reflns_limit_h_min              0
_reflns_limit_k_max              24
_reflns_limit_k_min              1
_reflns_limit_l_max              9
_reflns_limit_l_min              -9
_reflns_number_gt                1375
_reflns_number_total             1477
_reflns_threshold_expression     I>=2u(I)
_computing_molecular_graphics    'Olex2 1.3-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.3-dev (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'


_refine_diff_density_max         0.2272
_refine_diff_density_min         -0.2533
_refine_diff_density_rms         0.0239
_refine_ls_d_res_high            0.5774
_refine_ls_d_res_low             5.2764
_refine_ls_goodness_of_fit_ref   1.1216
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    1
_refine_ls_number_parameters     70
_refine_ls_number_reflns         1477
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0162
_refine_ls_R_factor_gt           0.0145
_refine_ls_restrained_S_all      1.1216
_refine_ls_shift/su_max          0.0007
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0118P)²+0.0845P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0332
_refine_ls_wR_factor_ref         0.0338
_refine_special_details          
;
Refinement using NoSpherA2, an implementation of
 NOn-SPHERical Atom-form-factors in Olex2.
Please cite:
F. Kleemiss, H. Puschmann, O. Dolomanov, S.Grabowsky - to be published - 2020
NoSpherA2 implementation of HAR makes use of
 tailor-made aspherical atomic form factors calculated
on-the-fly from a Hirshfeld-partitioned electron density (ED) - not from
spherical-atom form factors.

The ED is calculated from a gaussian basis set single determinant SCF
wavefunction - either Hartree-Fock or DFT using selected funtionals
 - for a fragment of the crystal.
This fregment can be embedded in an electrostatic crystal field by employing cluster charges.
The following options were used:
   SOFTWARE:       ORCA
   PARTITIONING:   NoSpherA2
   INT ACCURACY:   High
   METHOD:         PBE
   BASIS SET:      def2-TZVPP
   CHARGE:         0
   MULTIPLICITY:   1
   DATE:           2020-06-19_12-42-38
;
_olex2_refinement_description    
;
1. Others
 Sof(C4)=Sof(O2)=FVAR(1)
;
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
O1 O 0.436229(12) 0.578735(12) 0.16464(3) 0.01560(4) Uani 1.000000 1 . . .
C1 C 0.469611(14) 0.541809(14) 0.33313(4) 0.01239(4) Uani 1.000000 1 . . .
C2 C 0.522277(15) 0.594862(14) 0.52678(4) 0.01402(4) Uani 1.000000 1 . . .
C3 C 0.552478(15) 0.552592(15) 0.69364(4) 0.01403(4) Uani 1.000000 1 . . .
C4 C 0.333333333333 0.666666666667 0.666666666667 0.02222(15) Uani 0.855(2) 6 S
T P
O2 O 0.333333333333 0.666666666667 0.46383(9) 0.03519(16) Uani 0.855(2) 3 S T P
H2 H 0.5396(3) 0.6685(3) 0.5475(9) 0.0317(12) Uani 1.000000 1 . . .
H3 H 0.5925(4) 0.5917(3) 0.8464(8) 0.0328(12) Uani 1.000000 1 . . .
H1 H 0.4645(4) 0.6468(4) 0.1793(10) 0.0319(14) Uani 1.000000 1 . . .


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C1 1.3764(3) . ?
O1 H1 0.963(6) . ?
C1 C2 1.3962(3) . ?
C1 C3 1.3940(3) 4_666 ?
C2 C3 1.3951(3) . ?
C2 H2 1.087(4) . ?
C3 H3 1.081(5) . ?
C4 O2 1.1550(5) 16_566 ?
C4 O2 1.1550(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
H1 O1 C1 111.8(3) . . ?
C2 C1 O1 122.338(19) . . ?
C3 C1 O1 117.361(19) 4_666 . ?
C3 C1 C2 120.292(19) 4_666 . ?
C3 C2 C1 119.475(19) . . ?
H2 C2 C1 120.3(3) . . ?
H2 C2 C3 120.2(3) . . ?
C2 C3 C1 120.23(2) . 4_666 ?
H3 C3 C1 118.8(2) . 4_666 ?
H3 C3 C2 121.0(2) . . ?
O2 C4 O2 180.0 16_566 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C1 C2 C3 178.79(2) . . . . ?
O1 C1 C3 C2 -178.838(19) . . 4_666 4_666 ?
C1 C2 C3 C1 0.13(2) . . . 4_666 ?
C1 C3 C2 C1 0.13(2) 4_666 . . . ?

# start Validation Reply Form
_vrf_PLAT927_Pau100m71           
;
PROBLEM: Reported and Calculated  wR2 Differ by .........    -0.0755 Check 
RESPONSE: Non-Spherical refinement, therefore wR2 from CheckCIF is wrong
;
_vrf_PLAT928_Pau100m71           
;
PROBLEM: Reported and Calculated    S value   Differ by .     -2.505 Check 
RESPONSE: Non-Spherical refinement, therefore S from CheckCIF is wrong
;
_vrf_PLAT029_Pau100m71           
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.953 Why?  
RESPONSE: Data was used as published and deposited.
;
_vrf_PLAT926_Pau100m71           
;
PROBLEM: Reported and Calculated   R1 Differ by .........    -0.0238 Check 
RESPONSE: Non-Spherical refinement, therefore R1 from CheckCIF is wrong
;
# end Validation Reply Form


_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_GlyAla_12K_NoSpherA2_ORCA_NoSpherA2
_database_code_depnum_ccdc_archive 'CCDC 2035148'
loop_
_audit_author_name
_audit_author_address
'Florian Kleemiss'
;University of Bern
Switzerland
;
_audit_update_record             
;
2020-10-02 deposited with the CCDC.	2020-11-09 downloaded from the CCDC.
;

_audit_creation_date             2020-17-11
_audit_creation_method           
;
Olex2 1.3-dev
(compiled 2020.01.16 svn.ra754ea2f for OlexSys, GUI svn.r6014)
;

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        Glycil-L-Alanine
_chemical_name_common            Glycil-L-Alanine
_chemical_formula_moiety         'C5 H10 N2 O3'
_chemical_formula_sum            'C5 H10 N2 O3'
_chemical_formula_weight         146.1471
_chemical_absolute_configuration syn

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'p 21 21 21'
_symmetry_space_group_name_Hall  'p 2ac 2ab'
_symmetry_Int_Tables_number      19
loop_
_symmetry_equiv_pos_as_xyz
'+x, +y, +z'
'-x+1/2, -y, +z+1/2'
'+x+1/2, -y+1/2, -z'
'-x, +y+1/2, -z+1/2'

_cell_length_a                   7.4583(4)
_cell_length_b                   9.4892(7)
_cell_length_c                   9.7301(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     688.63(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    12(2)
_cell_measurement_reflns_used    276
_cell_measurement_theta_min      6.05
_cell_measurement_theta_max      21.1

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       Prismatic
_exptl_crystal_colour            Colourless
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_exptl_crystal_density_diffrn    1.41
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             312

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.071
_exptl_absorpt_correction_type   none

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      12(2)
_diffrn_radiation_wavelength     0.5259
_diffrn_radiation_type           synchrotron
_diffrn_radiation_monochromator  'Si(111) double crystal'
_diffrn_detector_area_resol_mean 0.657
_diffrn_measurement_device_type  'Bruker SMART-CCD'
_diffrn_measurement_method       'area detector'
_diffrn_reflns_av_R_equivalents  0.0253
_diffrn_reflns_av_unetI/netI     0.026
_diffrn_reflns_number            8493
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.57
_diffrn_reflns_theta_max         23.637
_diffrn_reflns_theta_full        18.393
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.976
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.969
_reflns_Friedel_fraction_full    0.986
_reflns_Friedel_fraction_max     0.958
_reflns_Friedel_coverage         0.711
_reflns_number_total             2394
_reflns_number_gt                2394
_reflns_threshold_expression     I/u(I)>2.1

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2008)'
_computing_structure_refinement  'olex2.refine 1.3-dev (Bourhis et al., 2015)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_hydrogens   difmap

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
_atom_type_scat_dispersion_source
H 0.00000 0.00000 'NoSPherA2 (see refine special details)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
C 0.00347 0.00161 'NoSPherA2 (see refine special details)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
O 0.01158 0.00611 'NoSPherA2 (see refine special details)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
N 0.00653 0.00323 'NoSPherA2 (see refine special details)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'

_refine_diff_density_max         0.1480
_refine_diff_density_min         -0.1877
_refine_diff_density_rms         0.0574
_refine_ls_abs_structure_details 
'Flack, H. D. (1983). Acta Cryst. A39, 876-881.'
_refine_ls_abs_structure_Flack   0.1(7)
_refine_ls_d_res_high            0.6558
_refine_ls_d_res_low             5.8638
_refine_ls_goodness_of_fit_ref   1.2843
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     181
_refine_ls_number_reflns         2374
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0158
_refine_ls_R_factor_gt           0.0158
_refine_ls_restrained_S_all      1.2843
_refine_ls_shift/su_max          0.0009
_refine_ls_shift/su_mean         0.0002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     w=1/[σ²(Fo²)]
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0308
_refine_ls_wR_factor_ref         0.0308

_refine_special_details          
;
Refinement using NoSpherA2, an implementation of 
NOn-SPHERical Atom-form-factors in Olex2.
Please cite:

F. Kleemiss, H. Puschmann, O. Dolomanov, S.Grabowsky - to be publsihed - 2020
NoSpherA2 makes use of tailor-made aspherical atomic form factors calculated
on-the-fly from a Hirshfeld-partitioned electron density (ED) - not from
spherical-atom form factors.

The ED is calculated from a gaussian basis set single determinant SCF
wavefunction - either Hartree-Fock or B3LYP 
- for a fragment of the crystal embedded in
an electrostatic crystal field.
The following options were used:
   SOFTWARE:       ORCA
   PARTITIONING:   NoSpherA2
   METHOD:         rhf
   BASIS SET:      6-311G(d,p)
   CHARGE:         0
   MULTIPLICITY:   1
   DATE:           2020-01-24_12-16-57
;
#----------------------------------------------------------------------------#
#                    VALIDATION REPLY FORM                                   #
#----------------------------------------------------------------------------#

# end Validation Reply Form

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_refinement_flags_posn
O(1) O -0.26775(4) -0.96250(3) -0.77796(3) 0.00568(5) Uani 1.000000 .
O(2) O -0.43046(4) -1.12553(3) -0.88361(3) 0.00505(6) Uani 1.000000 .
O(3) O -0.70877(4) -0.94883(3) -0.60022(3) 0.00539(5) Uani 1.000000 .
N(1) N -0.44247(4) -1.03635(4) -0.52555(3) 0.00374(6) Uani 1.000000 .
N(2) N -0.73417(4) -0.75564(4) -0.40093(3) 0.00412(6) Uani 1.000000 .
C(1) C -0.37319(5) -1.06533(4) -0.77671(3) 0.00331(6) Uani 1.000000 .
C(2) C -0.42592(5) -1.13472(4) -0.63921(3) 0.00359(6) Uani 1.000000 .
C(3) C -0.28337(6) -1.24507(4) -0.60454(4) 0.00787(7) Uani 1.000000 .
C(4) C -0.58862(5) -0.95479(4) -0.51389(3) 0.00346(6) Uani 1.000000 .
C(5) C -0.59817(5) -0.86705(4) -0.38208(4) 0.00465(7) Uani 1.000000 .
H(1) H -0.3550(9) -1.0420(9) -0.4483(7) 0.0214(18) Uani 1.000000 .
H(2a H -0.8615(9) -0.8016(9) -0.4084(9) 0.022(2) Uani 1.000000 .
H(2b H -0.7328(11) -0.6803(10) -0.3237(8) 0.0238(19) Uani 1.000000 .
H(2c H -0.7043(12) -0.7019(9) -0.4913(7) 0.0200(19) Uani 1.000000 .
H(2) H -0.5555(8) -1.1847(8) -0.6579(5) 0.0150(14) Uani 1.000000 .
H(3a H -0.1545(9) -1.1924(8) -0.5862(7) 0.0253(19) Uani 1.000000 .
H(3b H -0.3210(11) -1.3043(8) -0.5146(8) 0.0310(19) Uani 1.000000 .
H(3c H -0.2674(11) -1.3166(9) -0.6902(7) 0.0289(18) Uani 1.000000 .
H(5a H -0.4657(8) -0.8178(8) -0.3609(7) 0.0180(16) Uani 1.000000 .
H(5b H -0.6357(10) -0.9342(8) -0.2940(6) 0.0210(17) Uani 1.000000 .


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O(1) C(1) 1.2533(4) . ?
O(2) C(1) 1.2612(4) . ?
O(3) C(4) 1.2295(4) . ?
N(1) C(2) 1.4525(4) . ?
N(1) C(4) 1.3416(5) . ?
N(1) H(1) 0.997(6) . ?
N(2) C(5) 1.4765(5) . ?
N(2) H(2a 1.047(7) . ?
N(2) H(2b 1.037(9) . ?
N(2) H(2c 1.041(7) . ?
C(1) C(2) 1.5422(5) . ?
C(2) C(3) 1.5299(5) . ?
C(2) H(2) 1.092(6) . ?
C(3) H(3a 1.098(7) . ?
C(3) H(3b 1.077(8) . ?
C(3) H(3c 1.082(7) . ?
C(4) C(5) 1.5308(5) . ?
C(5) H(5a 1.112(6) . ?
C(5) H(5b 1.104(6) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C(4) N(1) C(2) 120.27(3) . . ?
H(1) N(1) C(2) 119.0(4) . . ?
H(1) N(1) C(4) 119.9(4) . . ?
H(2a N(2) C(5) 109.5(4) . . ?
H(2b N(2) C(5) 113.4(4) . . ?
H(2b N(2) H(2a 110.3(6) . . ?
H(2c N(2) C(5) 108.0(5) . . ?
H(2c N(2) H(2a 109.8(6) . . ?
H(2c N(2) H(2b 105.8(6) . . ?
O(2) C(1) O(1) 123.86(3) . . ?
C(2) C(1) O(1) 120.06(3) . . ?
C(2) C(1) O(2) 115.83(3) . . ?
C(1) C(2) N(1) 114.07(3) . . ?
C(3) C(2) N(1) 109.33(3) . . ?
C(3) C(2) C(1) 107.84(3) . . ?
H(2) C(2) N(1) 109.3(3) . . ?
H(2) C(2) C(1) 105.5(3) . . ?
H(2) C(2) C(3) 110.8(4) . . ?
H(3a C(3) C(2) 109.5(4) . . ?
H(3b C(3) C(2) 110.8(4) . . ?
H(3b C(3) H(3a 109.5(6) . . ?
H(3c C(3) C(2) 109.6(4) . . ?
H(3c C(3) H(3a 108.3(6) . . ?
H(3c C(3) H(3b 109.1(6) . . ?
N(1) C(4) O(3) 124.12(3) . . ?
C(5) C(4) O(3) 120.89(3) . . ?
C(5) C(4) N(1) 114.99(3) . . ?
C(4) C(5) N(2) 108.50(3) . . ?
H(5a C(5) N(2) 109.4(4) . . ?
H(5a C(5) C(4) 110.0(3) . . ?
H(5b C(5) N(2) 109.6(4) . . ?
H(5b C(5) C(4) 110.4(4) . . ?
H(5b C(5) H(5a 108.9(5) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O(1) C(1) C(2) N(1) 35.43(4) . . . . ?
O(1) C(1) C(2) C(3) -86.20(4) . . . . ?
O(2) C(1) C(2) N(1) -150.12(3) . . . . ?
O(2) C(1) C(2) C(3) 88.24(4) . . . . ?
O(3) C(4) N(1) C(2) -5.69(5) . . . . ?
O(3) C(4) C(5) N(2) -16.22(4) . . . . ?
N(1) C(4) C(5) N(2) 164.08(3) . . . . ?


# END of CIF
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_thpp
_database_code_depnum_ccdc_archive 'CCDC 2034387'
loop_
_audit_author_name
_audit_author_address
'Florian Kleemiss'
;University of Bern
Switzerland
;
_audit_update_record             
;
2020-09-28 deposited with the CCDC.	2020-11-09 downloaded from the CCDC.
;
_audit_creation_date             2020-03-13
_audit_creation_method           
;
Olex2 1.3-dev
(compiled 2020.03.04 svn.rc2590c38 for OlexSys, GUI svn.r6014)
;
_chemical_formula_moiety         'C10 H10 F2 N4'
_chemical_formula_sum            'C10 H10 F2 N4'
_chemical_formula_weight         224.215
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
_atom_type_scat_dispersion_source
H 0.00000 0.00000 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236
57.79970 0.0030380000826
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)' custom
C 0.00211 0.00161 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870
51.65120 0.215599998832
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)' custom
F 0.01364 0.01032 3.53920 2.64120 1.51700 1.02430 10.28250 4.29440 0.26150
26.14760 0.277599990368
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)' custom
N 0.00411 0.00331 12.21260 3.13220 2.01250 1.16630 0.00570 9.89330 28.99750
0.58260 -11.5290002823
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)' custom

_vrf_PLAT927_thpp                
;
PROBLEM: Reported and Calculated  wR2 Differ by .........    -0.0780 Check 
RESPONSE: Non-spherical refienment, therefore sattistics of ChecCIF are unreliable
;
_vrf_PLAT926_thpp                
;
PROBLEM: Reported and Calculated   R1 Differ by .........    -0.0255 Check 
RESPONSE: Non-spherical refienment, therefore sattistics of ChecCIF are unreliable
;
_vrf_PLAT928_thpp                
;
PROBLEM: Reported and Calculated    S value   Differ by .     -1.748 Check 
RESPONSE: Non-spherical refienment, therefore sattistics of ChecCIF are unreliable
;

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2ybc (x-z,y,z)'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x+1/2,y+1/2,-z+1/2
3 -x,-y,-z
4 x-1/2,-y-1/2,z-1/2

_symmetry_Int_Tables_number      14
_cell_length_a                   6.9196(1)
_cell_length_b                   14.5749(2)
_cell_length_c                   9.7248(1)
_cell_angle_alpha                90
_cell_angle_beta                 90.637(1)
_cell_angle_gamma                90
_cell_volume                     980.71(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    6303
_cell_measurement_theta_min      2.56
_cell_measurement_theta_max      30.96

_exptl_crystal_description       prism
_exptl_crystal_colour            'light yellow'
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.519
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             464
_exptl_absorpt_coefficient_mu    0.123
_exptl_absorpt_correction_type   none


_diffrn_ambient_temperature      120(2)
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART CCD 6000'
_diffrn_measurement_method       ω-scan
_diffrn_reflns_av_R_equivalents  0.0536
_diffrn_reflns_av_unetI/netI     0.0285
_diffrn_reflns_Laue_measured_fraction_full 1.0000
_diffrn_reflns_Laue_measured_fraction_max 1.0000
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            13911
_diffrn_reflns_point_group_measured_fraction_full 1.0000
_diffrn_reflns_point_group_measured_fraction_max 1.0000
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         2.52
_diffrn_measured_fraction_theta_full 1.0000
_diffrn_measured_fraction_theta_max 1.0000
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              8
_reflns_limit_h_min              -9
_reflns_limit_k_max              20
_reflns_limit_k_min              0
_reflns_limit_l_max              13
_reflns_limit_l_min              -7
_reflns_number_gt                2456
_reflns_number_total             2975
_reflns_threshold_expression     I>=2u(I)
_computing_molecular_graphics    'Olex2 1.3-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.3-dev (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.1588
_refine_diff_density_min         -0.2130
_refine_diff_density_rms         0.0591
_refine_ls_d_res_high            0.6999
_refine_ls_d_res_low             8.0891
_refine_ls_goodness_of_fit_ref   1.0794
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    3
_refine_ls_number_parameters     258
_refine_ls_number_reflns         2975
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0288
_refine_ls_R_factor_gt           0.0214
_refine_ls_restrained_S_all      1.0794
_refine_ls_shift/su_max          0.0003
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0177P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0454
_refine_ls_wR_factor_ref         0.0483
_refine_special_details          
;
Refinement using NoSpherA2, an implementation of 
NOn-SPHERical Atom-form-factors in Olex2.
Please cite:

F. Kleemiss, H. Puschmann, O. Dolomanov, S.Grabowsky - to be published - 2020
NoSpherA2 implementation of HAR makes use of tailor-made 
aspherical atomic form factors calculated
on-the-fly from a Hirshfeld-partitioned electron density (ED) - not from
spherical-atom form factors.

The ED is calculated from a gaussian basis set single determinant SCF
wavefunction - either Hartree-Fock or DFT using selected funtionals 
- for a fragment of the crystal.
This fregment can be embedded in an electrostatic crystal field by 
employing cluster charges.
The following options were used:
   SOFTWARE:       ORCA
   PARTITIONING:   NoSpherA2
   INT ACCURACY:   High
   METHOD:         PBE
   BASIS SET:      def2-TZVPP
   CHARGE:         0
   MULTIPLICITY:   1
   DATE:           2020-03-13_10-35-56
;
_olex2_refinement_description    
;
1. Others
 Sof(C00h)=Sof(H00k)=Sof(H00l)=Sof(C1)=Sof(H1b)=Sof(H1a)=1-FVAR(1)
 Sof(C00F)=Sof(H00g)=Sof(H00h)=Sof(C00G)=Sof(H00i)=Sof(H00j)=FVAR(1)
2.a Secondary CH2 refined with fixed occupancy and ADP/Uiso:
 C00h(H00k,H00l), C1(H1b,H1a)
;
_atom_sites_solution_primary     dual
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_refinement_flags_posn
_atom_site_disorder_group
F001 F 0.16752(4) 0.57360(2) 0.26258(3) 0.02707(8) Uani 1.000000 . .
F002 F 0.13120(5) 0.68497(2) 0.48746(4) 0.02902(8) Uani 1.000000 . .
N003 N 0.22200(6) 0.56957(3) 0.62956(4) 0.02008(9) Uani 1.000000 . .
N004 N 0.36182(6) 0.33061(3) 0.57637(4) 0.02014(9) Uani 1.000000 . .
N005 N 0.30290(6) 0.45756(3) 0.78542(4) 0.02393(10) Uani 1.000000 . .
N006 N 0.25111(8) 0.36110(4) 0.18032(5) 0.03649(12) Uani 1.000000 . .
C007 C 0.30117(6) 0.41737(3) 0.54235(5) 0.01663(9) Uani 1.000000 . .
C008 C 0.26225(6) 0.45015(3) 0.40935(5) 0.01793(10) Uani 1.000000 . .
C009 C 0.18832(7) 0.59752(3) 0.50240(5) 0.01999(10) Uani 1.000000 . .
C00A C 0.20611(7) 0.54280(3) 0.39025(5) 0.01943(10) Uani 1.000000 . .
C00B C 0.27489(6) 0.48319(3) 0.65269(5) 0.01782(10) Uani 1.000000 . .
C00C C 0.26097(8) 0.39696(4) 0.28619(5) 0.02432(11) Uani 1.000000 . .
C00D C 0.39577(9) 0.26085(4) 0.47323(6) 0.02690(12) Uani 1.000000 . .
H00a H 0.2614(12) 0.2354(6) 0.4272(9) 0.053(2) Uani 1.000000 . .
H00b H 0.4839(11) 0.2892(5) 0.3912(8) 0.042(2) Uani 1.000000 . .
H00c H 0.4731(13) 0.2060(5) 0.5206(9) 0.056(2) Uani 1.000000 . .
C00E C 0.26827(10) 0.52381(4) 0.89396(6) 0.02819(12) Uani 1.000000 . .
H00d H 0.3635(13) 0.5828(5) 0.8859(9) 0.059(3) Uani 1.000000 . .
H00e H 0.1244(12) 0.5515(6) 0.8856(9) 0.059(2) Uani 1.000000 . .
H00f H 0.2912(14) 0.4918(6) 0.9914(9) 0.068(3) Uani 1.000000 . .
C00F C 0.3680(3) 0.36581(8) 0.82064(13) 0.0241(2) Uani 0.882(5) . 1
H00g H 0.5260(13) 0.3652(6) 0.8300(9) 0.047(3) Uani 0.882(5) . 1
H00h H 0.3132(19) 0.3470(6) 0.9204(9) 0.045(5) Uani 0.882(5) . 1
C00G C 0.3055(3) 0.29777(5) 0.71192(7) 0.0241(3) Uani 0.882(5) . 1
H00i H 0.1456(13) 0.2875(6) 0.7156(9) 0.043(2) Uani 0.882(5) . 1
H00j H 0.3785(13) 0.2322(9) 0.7305(9) 0.042(10) Uani 0.882(5) . 1
H1a H 0.157(2) 0.3463(6) 0.8178(10) 0.053(19) Uiso 0.118(5) . 2
C1 C 0.292(2) 0.3652(6) 0.8186(10) 0.0256(18) Uani 0.118(5) . 2
H1b H 0.343(2) 0.3559(6) 0.9108(10) 0.12(9) Uiso 0.118(5) . 2
H00l H 0.5424(17) 0.3129(3) 0.7348(5) 0.031(14) Uiso 0.118(5) . 2
H00k H 0.3724(17) 0.2417(3) 0.7315(5) 0.06(10) Uiso 0.118(5) . 2
C00h C 0.4050(17) 0.3057(3) 0.7173(5) 0.0192(16) Uani 0.118(5) . 2


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
F001 C00A 1.3442(6) . ?
F002 C009 1.3418(5) . ?
N003 C009 1.3202(6) . ?
N003 C00B 1.3296(6) . ?
N004 C007 1.3716(6) . ?
N004 C00D 1.4492(7) . ?
N004 C00G 1.4594(8) . ?
N004 C00h 1.446(5) . ?
N005 C00B 1.3556(6) . ?
N005 C00E 1.4524(7) . ?
N005 C00F 1.4509(13) . ?
N005 C1 1.386(9) . ?
N006 C00C 1.1560(7) . ?
C007 C008 1.4022(7) . ?
C007 C00B 1.4523(7) . ?
C008 C00A 1.4167(7) . ?
C008 C00C 1.4267(7) . ?
C009 C00A 1.3578(7) . ?
C00D H00a 1.092(8) . ?
C00D H00b 1.091(7) . ?
C00D H00c 1.064(7) . ?
C00E H00d 1.087(8) . ?
C00E H00e 1.076(8) . ?
C00E H00f 1.066(9) . ?
C00F H00g 1.096(9) . ?
C00F H00h 1.081(10) . ?
C00F C00G 1.5093(17) . ?
C00G H00i 1.118(9) . ?
C00G H00j 1.095(13) . ?
H1a C1 0.9700 . ?
C1 H1b 0.9700 . ?
C1 C00h 1.534(12) . ?
H00l C00h 0.9700 . ?
H00k C00h 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C00B N003 C009 119.74(4) . . ?
C00D N004 C007 122.10(4) . . ?
C00G N004 C007 115.86(5) . . ?
C00G N004 C00D 116.23(5) . . ?
C00h N004 C007 121.33(18) . . ?
C00h N004 C00D 116.49(19) . . ?
C00h N004 C00G 27.8(4) . . ?
C00E N005 C00B 119.06(4) . . ?
C00F N005 C00B 121.30(6) . . ?
C00F N005 C00E 119.64(6) . . ?
C1 N005 C00B 118.8(4) . . ?
C1 N005 C00E 117.8(4) . . ?
C1 N005 C00F 21.3(5) . . ?
C008 C007 N004 126.28(4) . . ?
C00B C007 N004 118.11(4) . . ?
C00B C007 C008 115.60(4) . . ?
C00A C008 C007 119.69(4) . . ?
C00C C008 C007 126.05(5) . . ?
C00C C008 C00A 114.13(4) . . ?
N003 C009 F002 116.31(4) . . ?
C00A C009 F002 120.01(5) . . ?
C00A C009 N003 123.68(5) . . ?
C008 C00A F001 119.39(4) . . ?
C009 C00A F001 121.80(4) . . ?
C009 C00A C008 118.80(5) . . ?
N005 C00B N003 117.27(4) . . ?
C007 C00B N003 122.48(4) . . ?
C007 C00B N005 120.25(4) . . ?
C008 C00C N006 173.30(6) . . ?
H00a C00D N004 112.2(4) . . ?
H00b C00D N004 109.7(4) . . ?
H00b C00D H00a 108.0(6) . . ?
H00c C00D N004 108.2(4) . . ?
H00c C00D H00a 110.1(7) . . ?
H00c C00D H00b 108.6(6) . . ?
H00d C00E N005 111.6(4) . . ?
H00e C00E N005 110.7(5) . . ?
H00e C00E H00d 105.0(7) . . ?
H00f C00E N005 109.3(5) . . ?
H00f C00E H00d 109.0(7) . . ?
H00f C00E H00e 111.0(7) . . ?
H00g C00F N005 109.5(4) . . ?
H00h C00F N005 109.6(5) . . ?
H00h C00F H00g 106.4(8) . . ?
C00G C00F N005 110.76(10) . . ?
C00G C00F H00g 109.3(5) . . ?
C00G C00F H00h 111.2(6) . . ?
C00F C00G N004 109.88(11) . . ?
H00i C00G N004 110.3(5) . . ?
H00i C00G C00F 110.0(5) . . ?
H00j C00G N004 108.0(5) . . ?
H00j C00G C00F 109.2(5) . . ?
H00j C00G H00i 109.4(7) . . ?
H1a C1 N005 109.3(6) . . ?
H1b C1 N005 109.3(5) . . ?
H1b C1 H1a 107.94273350(2) . . ?
C00h C1 N005 111.7(7) . . ?
C00h C1 H1a 109.3(8) . . ?
C00h C1 H1b 109.3(6) . . ?
C1 C00h N004 111.4(7) . . ?
H00l C00h N004 109.3(5) . . ?
H00l C00h C1 109.3(9) . . ?
H00k C00h N004 109.3(3) . . ?
H00k C00h C1 109.3(6) . . ?
H00k C00h H00l 108.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
F001 C00A C008 C007 -179.47(4) . . . . ?
F001 C00A C008 C00C -3.36(5) . . . . ?
F001 C00A C009 F002 -0.13(5) . . . . ?
F001 C00A C009 N003 178.96(4) . . . . ?
F002 C009 N003 C00B 178.50(4) . . . . ?
F002 C009 C00A C008 -178.52(4) . . . . ?
N003 C009 C00A C008 0.56(6) . . . . ?
N003 C00B N005 C00E 1.93(6) . . . . ?
N003 C00B N005 C00F -177.57(9) . . . . ?
N003 C00B N005 C1 158.0(6) . . . . ?
N003 C00B C007 N004 178.00(4) . . . . ?
N003 C00B C007 C008 -1.57(5) . . . . ?
N004 C007 C008 C00A -178.05(5) . . . . ?
N004 C007 C008 C00C 6.33(6) . . . . ?
N004 C007 C00B N005 -2.49(5) . . . . ?
N004 C00G C00F N005 51.22(10) . . . . ?
N004 C00h C1 N005 -47.2(6) . . . . ?
N005 C00B C007 C008 177.94(4) . . . . ?
C007 C008 C00A C009 -1.04(5) . . . . ?


_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Os_PBE
_database_code_depnum_ccdc_archive 'CCDC 2034388'
loop_
_audit_author_name
_audit_author_address
'Florian Kleemiss'
;University of Bern
Switzerland
;
_audit_update_record             
;
2020-09-28 deposited with the CCDC.	2020-11-09 downloaded from the CCDC.
;
_audit_creation_date             2020-03-12
_audit_creation_method           
;
Olex2 1.3-dev
(compiled 2020.03.04 svn.rc2590c38 for OlexSys, GUI svn.r6014)
;
_chemical_formula_moiety         'C24 H44 Os P2'
_chemical_formula_sum            'C24 H44 Os P2'
_chemical_formula_weight         584.789
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
_atom_type_scat_dispersion_source
H 0.00000 0.00000 NoSpherA2
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
C 0.00347 0.00161 NoSpherA2
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
Os -1.02940 7.59418 NoSpherA2
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
P 0.10434 0.09671 NoSpherA2
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'

_vrf_PLAT974_Os_PBE              
;
PROBLEM: Check Calcd Negative Resid. Density on        Os      -5.13 eA-3  
RESPONSE: Non-spherical refienment, therefore sattistics of ChecCIF are unreliable
;
_vrf_PLAT910_Os_PBE              
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         11 Note  
RESPONSE: Reflections were affected by the Beamstop
;
_vrf_PLAT926_Os_PBE              
;
PROBLEM: Reported and Calculated   R1 Differ by .........    -0.0056 Check 
RESPONSE: Non-spherical refienment, therefore sattistics of ChecCIF are unreliable
;
_vrf_PLAT927_Os_PBE              
;
PROBLEM: Reported and Calculated  wR2 Differ by .........    -0.0105 Check 
RESPONSE: Non-spherical refienment, therefore sattistics of ChecCIF are unreliable
;
_vrf_PLAT928_Os_PBE              
;
PROBLEM: Reported and Calculated    S value   Differ by .     -0.380 Check 
RESPONSE: Non-spherical refienment, therefore sattistics of ChecCIF are unreliable
;

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2ybc (x-z,y,z)'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x+1/2,y+1/2,-z+1/2
3 -x,-y,-z
4 x-1/2,-y-1/2,z-1/2

_symmetry_Int_Tables_number      14
_cell_length_a                   10.8918(1)
_cell_length_b                   13.7619(1)
_cell_length_c                   17.0714(2)
_cell_angle_alpha                90
_cell_angle_beta                 98.563(1)
_cell_angle_gamma                90
_cell_volume                     2530.34(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    63613
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      36.3840
_cell_measurement_theta_min      3.5970
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.262
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.7c (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_coefficient_mu    5.176
_exptl_crystal_density_diffrn    1.535
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1176
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-3 -5 -2 0.1060
3 5 4 0.1078
-1 -1 5 0.0665
-3 -5 -4 0.1078
1 1 -5 0.0435
5 0 1 0.1557
-5 0 -1 0.1557
2 -5 -2 0.1561
-2 5 2 0.1561
3 5 2 0.1060

_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.212
_exptl_crystal_size_min          0.11
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-3.0094 -5.0063 -1.9870 -0.3272 -0.0417 -0.0951
3.0116 5.0110 3.9860 0.3427 0.1235 0.1067
-0.9962 -0.9887 5.0010 -0.0336 0.2137 -0.0122
-3.0116 -5.0110 -3.9860 -0.3427 -0.1235 -0.1067
0.9962 0.9887 -5.0010 0.0336 -0.2137 0.0122
5.0045 0.0045 0.9853 0.1335 0.0246 0.3098
-5.0045 -0.0045 -0.9853 -0.1335 -0.0246 -0.3098
1.9940 -5.0041 -2.0012 -0.2015 -0.0580 0.2090
-1.9940 5.0041 2.0012 0.2015 0.0580 -0.2090
3.0094 5.0063 1.9870 0.3272 0.0417 0.0951

_diffrn_reflns_av_R_equivalents  0.0582
_diffrn_reflns_av_unetI/netI     0.0248
_diffrn_reflns_Laue_measured_fraction_full 0.9976
_diffrn_reflns_Laue_measured_fraction_max 0.9986
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            196209
_diffrn_reflns_point_group_measured_fraction_full 0.9976
_diffrn_reflns_point_group_measured_fraction_max 0.9986
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         3.51
_diffrn_measured_fraction_theta_full 0.9976
_diffrn_measured_fraction_theta_max 0.9986
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              12
_reflns_limit_h_min              -15
_reflns_limit_k_max              19
_reflns_limit_k_min              0
_reflns_limit_l_max              24
_reflns_limit_l_min              -11
_reflns_number_gt                7199
_reflns_number_total             7723
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0856
_diffrn_detector_type            EosS2
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     50.00 105.00   1.00    3.65    --   36.08 159.00  95.00   55
  2  ω      9.00 104.00   1.00    3.65    --   36.08  77.00   0.00   95
  3  ω     19.00 103.00   1.00    3.65    --   36.08  57.00-180.00   84
  4  ω     35.00 108.00   1.00    3.65    --   36.08 178.00 150.00   73
  5  ω     35.00 108.00   1.00    3.65    --   36.08 178.00  30.00   73
  6  ω      9.00 104.00   1.00    3.65    --   36.08  77.00  60.00   95
  7  ω    -33.00 105.00   1.00    3.65    --   36.08   0.00-180.00  138
  8  ω    -33.00 105.00   1.00    3.65    --   36.08   0.00  60.00  138
  9  ω     -4.00  86.00   1.00    3.65    --   36.08-118.00-143.00   90
 10  ω     35.00 108.00   1.00    3.65    --   36.08 178.00-150.00   73
 11  ω      9.00 104.00   1.00    3.65    --   36.08  77.00-180.00   95
 12  ω      9.00 104.00   1.00    3.65    --   36.08  77.00 -90.00   95
 13  ω      9.00 104.00   1.00    3.65    --   36.08  77.00 120.00   95
 14  ω     19.00 103.00   1.00    3.65    --   36.08  57.00 -90.00   84
 15  ω    -99.00 -11.00   1.00    3.65    --  -30.00 -38.00 -30.00   88
 16  ω    -99.00 -11.00   1.00    3.65    --  -30.00 -38.00 150.00   88
 17  ω    -31.00  63.00   1.00    3.65    --   36.08 -77.00  60.00   94
 18  ω      9.00 104.00   1.00    3.65    --   36.08  77.00 -30.00   95
 19  ω     35.00 108.00   1.00    3.65    --   36.08 178.00 -30.00   73
 20  ω     20.00 109.00   1.00    3.65    --   36.08-159.00  63.00   89
 21  ω    -98.00  -3.00   1.00    3.65    --  -30.00 -77.00 150.00   95
 22  ω    -98.00  -3.00   1.00    3.65    --  -30.00 -77.00  30.00   95
 23  ω    -97.00 -13.00   1.00    3.65    --  -30.00 -57.00-150.00   84
 24  ω    -49.00  39.00   1.00    3.65    --  -30.00  38.00-120.00   88
 25  ω    -97.00 -19.00   1.00    3.65    --  -30.00 -57.00  30.00   78
 26  ω      9.00 104.00   1.00    3.65    --   36.08  77.00-150.00   95
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0251251000
_diffrn_orient_matrix_UB_12      0.0472240000
_diffrn_orient_matrix_UB_13      0.0076280000
_diffrn_orient_matrix_UB_21      -0.0031394000
_diffrn_orient_matrix_UB_22      -0.0060278000
_diffrn_orient_matrix_UB_23      0.0409225000
_diffrn_orient_matrix_UB_31      0.0607998000
_diffrn_orient_matrix_UB_32      -0.0198267000
_diffrn_orient_matrix_UB_33      0.0057471000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_special_details          
;
Refinement using NoSpherA2, an implementation of 
NOn-SPHERical Atom-form-factors in Olex2.
Please cite:

F. Kleemiss, H. Puschmann, O. Dolomanov, S.Grabowsky - to be publsihed - 2020
NoSpherA2 makes use of tailor-made aspherical atomic form factors calculated
on-the-fly from a Hirshfeld-partitioned electron density (ED) - not from
spherical-atom form factors.

The ED is calculated from a gaussian basis set single determinant SCF
wavefunction - either Hartree-Fock or DFT 
- for a fragment of the crystal embedded in
an electrostatic crystal field.
The following options were used:
   SOFTWARE:       ORCA
   PARTITIONING:   NoSpherA2
   METHOD:         PBE
   INT ACCURACY:   High
   BASIS SET:      x2c-TZVPP
   CHARGE:         0
   MULTIPLICITY:   1
   DATE:           2020-03-13_12-39-10
;
_computing_cell_refinement       'CrysAlisPro 1.171.39.7c (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.7c (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.7c (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-dev (Dolomanov et al., 2009)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_computing_structure_refinement  'olex2.refine 1.3-dev (Bourhis et al., 2015)'
_reflns_threshold_expression     I>=2u(I)
_refine_diff_density_max         0.5047
_refine_diff_density_min         -0.5003
_refine_diff_density_rms         0.0793
_refine_ls_d_res_high            0.7000
_refine_ls_d_res_low             5.7986
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_goodness_of_fit_ref   1.0722
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     636
_refine_ls_number_reflns         7723
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0143
_refine_ls_R_factor_gt           0.0119
_refine_ls_restrained_S_all      1.0717
_refine_ls_shift/su_max          0.0003
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0005P)²+0.2531P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0185
_refine_ls_wR_factor_ref         0.0189
_olex2_refinement_description    
;
1. Rigid body (RIGU) restrains
 H8, Os
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 H7, Os
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
;
_atom_sites_solution_primary     dual
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
P002 P 0.64836(2) 0.598594(18) 0.200797(15) 0.01276(5) Uani 1.000000 . .
P003 P 0.33818(2) 0.406082(18) 0.268430(15) 0.01251(5) Uani 1.000000 . .
C004 C 0.37841(9) 0.32778(7) 0.35559(6) 0.0159(2) Uani 1.000000 . .
C005 C 0.30571(10) 0.31745(8) 0.18632(6) 0.0181(2) Uani 1.000000 . .
C006 C 0.76659(10) 0.65205(8) 0.27749(7) 0.0186(2) Uani 1.000000 . .
C007 C 0.61739(9) 0.69827(7) 0.12930(6) 0.0156(2) Uani 1.000000 . .
C008 C 0.73932(10) 0.51139(7) 0.14854(7) 0.0186(2) Uani 1.000000 . .
C009 C 0.33192(11) 0.23311(8) 0.35882(7) 0.0198(2) Uani 1.000000 . .
C00A C 0.25019(15) 0.36648(10) 0.10853(8) 0.0298(3) Uani 1.000000 . .
C00B C 0.50071(11) 0.70520(8) 0.08316(6) 0.0194(2) Uani 1.000000 . .
C00C C 0.18089(10) 0.45036(8) 0.28141(7) 0.0202(2) Uani 1.000000 . .
C00D C 0.82254(14) 0.57581(10) 0.33744(9) 0.0291(3) Uani 1.000000 . .
C00E C 0.70657(12) 0.76883(8) 0.11930(7) 0.0219(2) Uani 1.000000 . .
C00F C 0.45240(11) 0.36467(9) 0.42293(7) 0.0247(2) Uani 1.000000 . .
C00G C 0.66231(13) 0.47373(10) 0.07233(7) 0.0251(2) Uani 1.000000 . .
C00H C 0.67815(12) 0.84544(8) 0.06641(7) 0.0261(3) Uani 1.000000 . .
C00I C 0.71497(13) 0.73711(9) 0.32002(8) 0.0247(3) Uani 1.000000 . .
C00J C 0.56035(13) 0.85269(8) 0.02266(7) 0.0269(3) Uani 1.000000 . .
C00K C 0.07854(12) 0.37350(9) 0.26791(10) 0.0260(3) Uani 1.000000 . .
C00L C 0.35925(11) 0.17718(9) 0.42723(7) 0.0245(2) Uani 1.000000 . .
C00M C 0.42150(13) 0.25935(10) 0.17563(9) 0.0278(3) Uani 1.000000 . .
C00N C 0.18281(14) 0.49646(11) 0.36308(10) 0.0317(3) Uani 1.000000 . .
C00O C 0.47182(12) 0.78187(9) 0.03019(7) 0.0257(3) Uani 1.000000 . .
C00P C 0.43237(12) 0.21515(9) 0.49388(8) 0.0286(3) Uani 1.000000 . .
C00Q C 0.47864(13) 0.30928(10) 0.49169(8) 0.0321(3) Uani 1.000000 . .
C00R C 0.86358(13) 0.55063(10) 0.13037(10) 0.0305(3) Uani 1.000000 . .
H00i H 0.7977(13) 0.7668(10) 0.1537(10) 0.051(5) Uani 1.000000 . .
H00n H 0.7477(14) 0.8991(11) 0.0601(9) 0.055(5) Uani 1.000000 . .
H00r H 0.5389(15) 0.9150(11) -0.0163(9) 0.060(5) Uani 1.000000 . .
H00 H 0.3792(13) 0.7860(10) -0.0042(8) 0.043(4) Uani 1.000000 . .
H00d H 0.4313(12) 0.6524(10) 0.0907(8) 0.034(4) Uani 1.000000 . .
H00j H 0.4913(14) 0.4360(11) 0.4183(8) 0.047(4) Uani 1.000000 . .
H2 H 0.5331(15) 0.3405(12) 0.5426(9) 0.066(6) Uani 1.000000 . .
H1 H 0.4534(14) 0.1722(11) 0.5471(9) 0.055(5) Uani 1.000000 . .
H00v H 0.3237(14) 0.1037(11) 0.4283(9) 0.057(5) Uani 1.000000 . .
H009 H 0.2738(14) 0.2029(11) 0.3081(8) 0.051(5) Uani 1.000000 . .
H005 H 0.2356(11) 0.2665(9) 0.2034(8) 0.029(4) Uani 1.000000 . .
H006 H 0.8423(13) 0.6807(10) 0.2457(8) 0.037(4) Uani 1.000000 . .
H008 H 0.7590(13) 0.4513(9) 0.1912(8) 0.033(4) Uani 1.000000 . .
H00a H 0.1678(15) 0.4073(13) 0.1152(9) 0.058(5) Uani 1.000000 . .
H00b H 0.3184(16) 0.4138(13) 0.0868(9) 0.062(5) Uani 1.000000 . .
H00c H 0.2247(17) 0.3095(13) 0.0634(9) 0.071(6) Uani 1.000000 . .
H00e H 0.1614(12) 0.5072(10) 0.2369(9) 0.036(4) Uani 1.000000 . .
H00f H 0.7525(15) 0.5517(13) 0.3716(10) 0.063(6) Uani 1.000000 . .
H00g H 0.8557(16) 0.5129(11) 0.3095(11) 0.067(6) Uani 1.000000 . .
H00h H 0.8993(13) 0.6072(11) 0.3776(9) 0.052(5) Uani 1.000000 . .
H00k H 0.5767(15) 0.4401(11) 0.0827(9) 0.056(5) Uani 1.000000 . .
H00l H 0.6390(15) 0.5324(11) 0.0304(9) 0.050(5) Uani 1.000000 . .
H00m H 0.7176(14) 0.4190(11) 0.0458(9) 0.051(5) Uani 1.000000 . .
H00o H 0.6698(13) 0.7927(9) 0.2795(8) 0.039(4) Uani 1.000000 . .
H00p H 0.6476(14) 0.7139(11) 0.3562(10) 0.055(5) Uani 1.000000 . .
H00q H 0.7895(14) 0.7706(11) 0.3605(9) 0.051(5) Uani 1.000000 . .
H00s H 0.0615(14) 0.3480(13) 0.2074(10) 0.059(5) Uani 1.000000 . .
H00t H 0.1013(14) 0.3126(11) 0.3045(10) 0.052(5) Uani 1.000000 . .
H00u H -0.0087(14) 0.4036(12) 0.2813(11) 0.060(5) Uani 1.000000 . .
H00w H 0.4919(15) 0.3054(12) 0.1618(10) 0.062(5) Uani 1.000000 . .
H00x H 0.4586(15) 0.2209(12) 0.2296(9) 0.057(5) Uani 1.000000 . .
H00y H 0.3978(15) 0.2068(11) 0.1270(9) 0.058(5) Uani 1.000000 . .
H00z H 0.1983(16) 0.4412(13) 0.4095(10) 0.065(6) Uani 1.000000 . .
H H 0.2543(15) 0.5513(12) 0.3755(9) 0.052(5) Uani 1.000000 . .
Ha H 0.0915(15) 0.5301(12) 0.3639(10) 0.063(5) Uani 1.000000 . .
H3 H 0.8496(14) 0.6137(11) 0.0899(10) 0.055(5) Uani 1.000000 . .
Hb H 0.9257(13) 0.5718(12) 0.1823(10) 0.049(5) Uani 1.000000 . .
Hc H 0.9123(14) 0.4952(11) 0.1021(10) 0.056(5) Uani 1.000000 . .
Os Os 0.478328(4) 0.530020(3) 0.249003(2) 0.015000(14) Uani 1.000000 . U
H5 H 0.3928(18) 0.5758(15) 0.3067(12) 0.096(7) Uani 1.000000 . .
H9 H 0.5503(14) 0.5299(13) 0.3320(11) 0.077(6) Uani 1.000000 . .
H4 H 0.4857(12) 0.6435(10) 0.2649(8) 0.031(4) Uiso 1.000000 . .
H7 H 0.4600(14) 0.4824(10) 0.1673(8) 0.048(5) Uani 1.000000 . U
H8 H 0.5685(13) 0.4421(10) 0.2606(10) 0.053(5) Uani 1.000000 . U
H6 H 0.3709(12) 0.5782(11) 0.1905(9) 0.051(5) Uani 1.000000 . .


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P002 C006 1.8470(11) . ?
P002 C007 1.8337(10) . ?
P002 C008 1.8657(11) . ?
P002 Os 2.3348(3) . ?
P003 C004 1.8366(10) . ?
P003 C005 1.8520(11) . ?
P003 C00C 1.8624(11) . ?
P003 Os 2.3452(3) . ?
C004 C009 1.4019(14) . ?
C004 C00F 1.3973(15) . ?
C005 C00A 1.5315(17) . ?
C005 C00M 1.5270(17) . ?
C005 H005 1.108(13) . ?
C006 C00D 1.5277(16) . ?
C006 C00I 1.5281(16) . ?
C006 H006 1.123(14) . ?
C007 C00B 1.3952(15) . ?
C007 C00E 1.4018(14) . ?
C008 C00G 1.5297(16) . ?
C008 C00R 1.5311(17) . ?
C008 H008 1.101(12) . ?
C009 C00L 1.3934(15) . ?
C009 H009 1.077(14) . ?
C00A H00a 1.079(17) . ?
C00A H00b 1.094(15) . ?
C00A H00c 1.105(15) . ?
C00B C00O 1.3947(15) . ?
C00B H00d 1.070(13) . ?
C00C C00K 1.5290(16) . ?
C00C C00N 1.5291(18) . ?
C00C H00e 1.089(13) . ?
C00D H00f 1.080(16) . ?
C00D H00g 1.076(16) . ?
C00D H00h 1.089(14) . ?
C00E C00H 1.3925(16) . ?
C00E H00i 1.076(14) . ?
C00F C00Q 1.3931(16) . ?
C00F H00j 1.077(14) . ?
C00G H00k 1.078(15) . ?
C00G H00l 1.083(15) . ?
C00G H00m 1.103(14) . ?
C00H C00J 1.3888(18) . ?
C00H H00n 1.075(14) . ?
C00I H00o 1.098(13) . ?
C00I H00p 1.076(15) . ?
C00I H00q 1.088(14) . ?
C00J C00O 1.3903(17) . ?
C00J H00r 1.089(14) . ?
C00K H00s 1.081(17) . ?
C00K H00t 1.054(16) . ?
C00K H00u 1.092(16) . ?
C00L C00P 1.3901(18) . ?
C00L H00v 1.084(15) . ?
C00M H00w 1.048(16) . ?
C00M H00x 1.088(15) . ?
C00M H00y 1.102(14) . ?
C00N H00z 1.093(17) . ?
C00N H 1.083(16) . ?
C00N Ha 1.099(15) . ?
C00O H00 1.090(13) . ?
C00P C00Q 1.3925(18) . ?
C00P H1 1.079(13) . ?
C00Q H2 1.067(15) . ?
C00R H3 1.106(16) . ?
C00R Hb 1.072(15) . ?
C00R Hc 1.083(15) . ?
Os H5 1.584(16) . ?
Os H9 1.513(17) . ?
Os H4 1.585(14) . ?
Os H7 1.527(14) . ?
Os H8 1.553(14) . ?
Os H6 1.568(14) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C007 P002 C006 102.34(5) . . ?
C008 P002 C006 103.37(5) . . ?
C008 P002 C007 102.77(5) . . ?
Os P002 C006 114.65(4) . . ?
Os P002 C007 117.39(3) . . ?
Os P002 C008 114.46(3) . . ?
C005 P003 C004 102.85(5) . . ?
C00C P003 C004 102.02(5) . . ?
C00C P003 C005 103.31(5) . . ?
Os P003 C004 117.35(3) . . ?
Os P003 C005 115.27(4) . . ?
Os P003 C00C 114.11(3) . . ?
C009 C004 P003 122.21(8) . . ?
C00F C004 P003 119.48(8) . . ?
C00F C004 C009 118.22(10) . . ?
C00A C005 P003 111.87(8) . . ?
C00M C005 P003 111.55(8) . . ?
C00M C005 C00A 110.70(11) . . ?
H005 C005 P003 106.2(6) . . ?
H005 C005 C00A 108.0(7) . . ?
H005 C005 C00M 108.3(6) . . ?
C00D C006 P002 111.58(8) . . ?
C00I C006 P002 112.02(8) . . ?
C00I C006 C00D 110.25(11) . . ?
H006 C006 P002 106.3(7) . . ?
H006 C006 C00D 108.4(7) . . ?
H006 C006 C00I 108.0(7) . . ?
C00B C007 P002 119.26(8) . . ?
C00E C007 P002 122.49(8) . . ?
C00E C007 C00B 118.25(10) . . ?
C00G C008 P002 111.20(8) . . ?
C00R C008 P002 114.73(8) . . ?
C00R C008 C00G 109.67(11) . . ?
H008 C008 P002 103.4(7) . . ?
H008 C008 C00G 109.6(7) . . ?
H008 C008 C00R 108.0(7) . . ?
C00L C009 C004 120.86(11) . . ?
H009 C009 C004 120.0(8) . . ?
H009 C009 C00L 119.2(8) . . ?
H00a C00A C005 111.4(9) . . ?
H00b C00A C005 110.8(8) . . ?
H00b C00A H00a 110.1(13) . . ?
H00c C00A C005 108.5(9) . . ?
H00c C00A H00a 108.5(12) . . ?
H00c C00A H00b 107.4(12) . . ?
C00O C00B C007 121.09(11) . . ?
H00d C00B C007 119.1(7) . . ?
H00d C00B C00O 119.7(7) . . ?
C00K C00C P003 114.75(8) . . ?
C00N C00C P003 110.88(9) . . ?
C00N C00C C00K 109.58(11) . . ?
H00e C00C P003 103.8(7) . . ?
H00e C00C C00K 109.2(7) . . ?
H00e C00C C00N 108.3(8) . . ?
H00f C00D C006 109.3(9) . . ?
H00g C00D C006 112.5(9) . . ?
H00g C00D H00f 107.6(13) . . ?
H00h C00D C006 110.0(8) . . ?
H00h C00D H00f 108.7(12) . . ?
H00h C00D H00g 108.7(12) . . ?
C00H C00E C007 120.82(11) . . ?
H00i C00E C007 121.0(8) . . ?
H00i C00E C00H 118.2(8) . . ?
C00Q C00F C004 121.01(11) . . ?
H00j C00F C004 117.1(7) . . ?
H00j C00F C00Q 121.8(7) . . ?
H00k C00G C008 112.5(8) . . ?
H00l C00G C008 110.7(8) . . ?
H00l C00G H00k 107.7(12) . . ?
H00m C00G C008 108.5(8) . . ?
H00m C00G H00k 108.3(11) . . ?
H00m C00G H00l 109.0(11) . . ?
C00J C00H C00E 120.09(11) . . ?
H00n C00H C00E 119.6(8) . . ?
H00n C00H C00J 120.4(8) . . ?
H00o C00I C006 113.4(7) . . ?
H00p C00I C006 112.1(8) . . ?
H00p C00I H00o 106.8(11) . . ?
H00q C00I C006 109.5(8) . . ?
H00q C00I H00o 109.1(11) . . ?
H00q C00I H00p 105.6(12) . . ?
C00O C00J C00H 119.86(11) . . ?
H00r C00J C00H 118.8(9) . . ?
H00r C00J C00O 121.3(9) . . ?
H00s C00K C00C 112.7(9) . . ?
H00t C00K C00C 111.1(8) . . ?
H00t C00K H00s 107.5(12) . . ?
H00u C00K C00C 110.1(8) . . ?
H00u C00K H00s 107.0(12) . . ?
H00u C00K H00t 108.2(12) . . ?
C00P C00L C009 120.22(11) . . ?
H00v C00L C009 119.8(8) . . ?
H00v C00L C00P 120.0(8) . . ?
H00w C00M C005 110.8(9) . . ?
H00x C00M C005 111.3(8) . . ?
H00x C00M H00w 107.0(13) . . ?
H00y C00M C005 109.2(9) . . ?
H00y C00M H00w 108.9(12) . . ?
H00y C00M H00x 109.6(12) . . ?
H00z C00N C00C 110.6(9) . . ?
H C00N C00C 112.3(8) . . ?
H C00N H00z 108.3(13) . . ?
Ha C00N C00C 107.3(10) . . ?
Ha C00N H00z 109.0(12) . . ?
Ha C00N H 109.2(12) . . ?
C00J C00O C00B 119.84(12) . . ?
H00 C00O C00B 119.3(8) . . ?
H00 C00O C00J 120.8(8) . . ?
C00Q C00P C00L 119.56(11) . . ?
H1 C00P C00L 120.4(9) . . ?
H1 C00P C00Q 120.0(9) . . ?
C00P C00Q C00F 120.13(12) . . ?
H2 C00Q C00F 119.1(9) . . ?
H2 C00Q C00P 120.8(9) . . ?
H3 C00R C008 111.1(8) . . ?
Hb C00R C008 113.4(8) . . ?
Hb C00R H3 108.3(12) . . ?
Hc C00R C008 110.4(8) . . ?
Hc C00R H3 107.8(12) . . ?
Hc C00R Hb 105.6(12) . . ?
P003 Os P002 155.635(9) . . ?
H5 Os P002 129.0(7) . . ?
H5 Os P003 75.3(7) . . ?
H9 Os P002 90.2(6) . . ?
H9 Os P003 97.1(6) . . ?
H9 Os H5 71.9(10) . . ?
H4 Os P002 68.9(5) . . ?
H4 Os P003 135.2(5) . . ?
H4 Os H5 61.4(8) . . ?
H4 Os H9 80.5(8) . . ?
H7 Os P002 81.6(5) . . ?
H7 Os P003 79.5(5) . . ?
H7 Os H5 136.9(10) . . ?
H7 Os H9 146.4(10) . . ?
H7 Os H4 125.2(7) . . ?
H8 Os P002 80.8(5) . . ?
H8 Os P003 80.1(5) . . ?
H8 Os H5 130.6(10) . . ?
H8 Os H9 69.5(9) . . ?
H8 Os H4 137.0(8) . . ?
H8 Os H7 77.0(9) . . ?
H6 Os P002 99.2(5) . . ?
H6 Os P003 87.6(5) . . ?
H6 Os H5 77.1(9) . . ?
H6 Os H9 146.1(10) . . ?
H6 Os H4 73.0(7) . . ?
H6 Os H7 67.4(8) . . ?
H6 Os H8 144.0(9) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
P002 C007 C00B C00O 177.61(9) . . . . ?
P002 C007 C00E C00H -177.68(9) . . . . ?
P003 C004 C009 C00L -176.83(9) . . . . ?
P003 C004 C00F C00Q 176.17(10) . . . . ?
C004 C009 C00L C00P 0.69(13) . . . . ?
C004 C00F C00Q C00P 0.83(15) . . . . ?
C007 C00B C00O C00J 0.24(13) . . . . ?
C007 C00E C00H C00J -0.07(13) . . . . ?
C009 C00L C00P C00Q -0.32(14) . . . . ?
C00B C00O C00J C00H 1.64(14) . . . . ?
C00E C00H C00J C00O -1.72(14) . . . . ?
C00F C00Q C00P C00L -0.43(16) . . . . ?


_olex2_submission_special_instructions 'No special instructions were received'
loop_
_restr_RIGU_atom_site_label_1
_restr_RIGU_atom_site_label_2
_restr_RIGU_target_weight_param
_restr_RIGU_U13_diff
_restr_RIGU_U23_diff
_restr_RIGU_U33_diff
Os H7 0.004000 -0.001104 0.008843 -0.013484
Os H8 0.004000 -0.002098 0.001392 -0.012715

