# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# 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. 
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data_cs148_150k
_audit_block_doi                 10.5517/ccdc.csd.cc2dhp2p
_database_code_depnum_ccdc_archive 'CCDC 2219602'
loop_
_citation_id
_citation_doi
_citation_year
1 10.26434/chemrxiv-2023-rcvdn 2023
_audit_update_record             
;
2024-01-23 deposited with the CCDC.	2024-05-06 downloaded from the CCDC.
;
_audit_creation_date             2023-11-14
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
carlotta.seno@unibas.ch
alessandro.prescimone@unibas.ch
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C36 H30 Cl4 O2 P2 Ti'
_chemical_formula_sum            'C36 H30 Cl4 O2 P2 Ti'
_chemical_formula_weight         746.24
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2191 1.8069 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.4279(3)
_cell_length_b                   9.5623(3)
_cell_length_c                   10.3638(3)
_cell_angle_alpha                102.086(2)
_cell_angle_beta                 108.255(2)
_cell_angle_gamma                92.847(2)
_cell_volume                     860.92(5)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    30055
_cell_measurement_temperature    150
_cell_measurement_theta_max      72.90
_cell_measurement_theta_min      4.63
_shelx_estimated_absorpt_T_max   0.581
_shelx_estimated_absorpt_T_min   0.335
_exptl_absorpt_coefficient_mu    6.096
_exptl_absorpt_correction_T_max  0.0006
_exptl_absorpt_correction_T_min  0.0000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens in: F. R. Ahmed (Editor), "Crystallographic Computing", Munksgaard,
Copenhagen (1970), 255 - 270. Afterwards scaling of reflection intensities was
performed within STOE LANA. J. Koziskova, F. Hahn, J. Richter, J. Kozisek, Acta
Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Finally a spherical absorption correction was done within STOE LANA.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.439
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             382
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-3 -5 30 0.1199
-19 -30 -22 0.1409
9 4 -15 0.1281
-15 8 10 0.3191
19 -16 30 0.2208
-30 5 -6 0.2027
23 30 22 0.1446
3 -2 -15 0.1482
30 5 -1 0.2191
-15 14 -15 0.2831
-15 -3 14 0.1795

_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.183
_exptl_crystal_size_min          0.1
_exptl_crystal_size_rad          0.170
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0453
_diffrn_reflns_av_unetI/netI     0.0297
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            15120
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         72.884
_diffrn_reflns_theta_min         4.625
_diffrn_ambient_temperature      150
_diffrn_detector                 'EIGER2 1M'
_diffrn_detector_area_resol_mean 13.33
_diffrn_detector_type            ?
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_details      
;
 3675 frames, detector distance = 40 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI Cu'
_diffrn_measurement_method       'rotation method, ω scans'
_diffrn_radiation_collimation    '1.2 0.6 mm diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  270
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54186
_diffrn_source                   'Axo Cu'
_diffrn_source_current           1.00
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3038
_reflns_number_total             3380
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'X-Area Recipe 1.37.0.0 (STOE, 2021)'
_computing_data_collection       'X-Area Pilatus3_SV 1.31.186.0 (STOE, 2022)'
_computing_data_reduction        
;
X-Area Integrate 2.5.3.0 (STOE, 2021)
X-Area LANA 2.7.5.0 (STOE, 2022)
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.716
_refine_diff_density_min         -0.720
_refine_diff_density_rms         0.105
_refine_ls_extinction_coef       0.0137(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   0.916
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     206
_refine_ls_number_reflns         3380
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0925
_refine_ls_R_factor_gt           0.0832
_refine_ls_restrained_S_all      0.916
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0800P)²+3.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1865
_refine_ls_wR_factor_ref         0.1991
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C8(H8), C6(H6), C12(H12), C14(H14), C11(H11), C3(H3), C18(H18),
 C10(H10), C4(H4), C5(H5), C9(H9), C17(H17), C15(H15), C16(H16)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti 0.500000 0.000000 0.000000 0.0600(4) Uani 1 2 d S . P . .
Cl1 Cl 0.67875(15) -0.14125(14) 0.09759(14) 0.0685(4) Uani 1 1 d . . . . .
Cl2 Cl 0.36050(15) -0.05037(15) 0.13914(14) 0.0699(4) Uani 1 1 d . . . . .
P1 P 0.73325(16) 0.27127(15) 0.25831(15) 0.0654(4) Uani 1 1 d . . . . .
O005 O 0.6086(4) 0.1674(4) 0.1449(4) 0.0669(9) Uani 1 1 d . . . . .
C13 C 0.6576(6) 0.4334(6) 0.3059(6) 0.0697(13) Uani 1 1 d . . . . .
C1 C 0.8876(6) 0.3103(6) 0.2002(6) 0.0675(13) Uani 1 1 d . . . . .
C7 C 0.8042(7) 0.1987(6) 0.4085(6) 0.0703(13) Uani 1 1 d . . . . .
C2 C 0.9571(7) 0.1959(6) 0.1492(7) 0.0751(15) Uani 1 1 d . . . . .
H2 H 0.920049 0.099657 0.143085 0.090 Uiso 1 1 calc R U . . .
C8 C 0.7043(7) 0.1157(7) 0.4451(6) 0.0779(15) Uani 1 1 d . . . . .
H8 H 0.601746 0.092503 0.387282 0.093 Uiso 1 1 calc R U . . .
C6 C 0.9425(7) 0.4506(6) 0.2090(7) 0.0770(15) Uani 1 1 d . . . . .
H6 H 0.894079 0.528945 0.240707 0.092 Uiso 1 1 calc R U . . .
C12 C 0.9572(7) 0.2280(6) 0.4907(6) 0.0783(15) Uani 1 1 d . . . . .
H12 H 1.026470 0.281856 0.464368 0.094 Uiso 1 1 calc R U . . .
C14 C 0.5587(7) 0.4843(6) 0.1997(7) 0.0750(15) Uani 1 1 d . . . . .
H14 H 0.531099 0.431163 0.105270 0.090 Uiso 1 1 calc R U . . .
C11 C 1.0057(8) 0.1763(7) 0.6123(6) 0.0837(18) Uani 1 1 d . . . . .
H11 H 1.108830 0.193799 0.668680 0.100 Uiso 1 1 calc R U . . .
C3 C 1.0769(7) 0.2216(7) 0.1087(7) 0.0804(16) Uani 1 1 d . . . . .
H3 H 1.121932 0.143078 0.071823 0.096 Uiso 1 1 calc R U . . .
C18 C 0.6965(7) 0.5105(7) 0.4445(7) 0.0789(16) Uani 1 1 d . . . . .
H18 H 0.761544 0.474370 0.517097 0.095 Uiso 1 1 calc R U . . .
C10 C 0.9034(8) 0.1002(7) 0.6499(7) 0.0843(18) Uani 1 1 d . . . . .
H10 H 0.936472 0.070179 0.735113 0.101 Uiso 1 1 calc R U . . .
C4 C 1.1349(8) 0.3620(7) 0.1205(7) 0.0864(17) Uani 1 1 d . . . . .
H4 H 1.220327 0.378990 0.093325 0.104 Uiso 1 1 calc R U . . .
C5 C 1.0693(8) 0.4757(7) 0.1711(8) 0.0898(19) Uani 1 1 d . . . . .
H5 H 1.109964 0.571627 0.180377 0.108 Uiso 1 1 calc R U . . .
C9 C 0.7565(8) 0.0668(7) 0.5681(7) 0.0842(17) Uani 1 1 d . . . . .
H9 H 0.689207 0.010328 0.594310 0.101 Uiso 1 1 calc R U . . .
C17 C 0.6395(8) 0.6418(7) 0.4771(8) 0.0882(18) Uani 1 1 d . . . . .
H17 H 0.666258 0.696166 0.571020 0.106 Uiso 1 1 calc R U . . .
C15 C 0.5003(8) 0.6130(6) 0.2322(8) 0.0830(17) Uani 1 1 d . . . . .
H15 H 0.431333 0.646867 0.160140 0.100 Uiso 1 1 calc R U . . .
C16 C 0.5421(8) 0.6900(7) 0.3669(8) 0.0892(19) Uani 1 1 d . . . . .
H16 H 0.504227 0.779272 0.387176 0.107 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Ti1 Cl1 2.3276(11) 2_655 ?
Ti1 Cl1 2.3276(11) . ?
Ti1 Cl2 2.3361(13) . ?
Ti1 Cl2 2.3361(13) 2_655 ?
Ti1 O005 1.932(4) . ?
Ti1 O005 1.932(4) 2_655 ?
P1 O005 1.510(4) . ?
P1 C13 1.780(6) . ?
P1 C1 1.791(6) . ?
P1 C7 1.789(6) . ?
C13 C14 1.394(8) . ?
C13 C18 1.393(8) . ?
C1 C2 1.397(8) . ?
C1 C6 1.388(8) . ?
C7 C8 1.391(8) . ?
C7 C12 1.405(8) . ?
C2 H2 0.9500 . ?
C2 C3 1.351(8) . ?
C8 H8 0.9500 . ?
C8 C9 1.403(8) . ?
C6 H6 0.9500 . ?
C6 C5 1.395(9) . ?
C12 H12 0.9500 . ?
C12 C11 1.401(8) . ?
C14 H14 0.9500 . ?
C14 C15 1.394(8) . ?
C11 H11 0.9500 . ?
C11 C10 1.377(10) . ?
C3 H3 0.9500 . ?
C3 C4 1.390(9) . ?
C18 H18 0.9500 . ?
C18 C17 1.408(8) . ?
C10 H10 0.9500 . ?
C10 C9 1.359(10) . ?
C4 H4 0.9500 . ?
C4 C5 1.368(9) . ?
C5 H5 0.9500 . ?
C9 H9 0.9500 . ?
C17 H17 0.9500 . ?
C17 C16 1.401(9) . ?
C15 H15 0.9500 . ?
C15 C16 1.358(10) . ?
C16 H16 0.9500 . ?

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
Cl1 Ti1 Cl1 180.0 2_655 . ?
Cl1 Ti1 Cl2 90.11(5) . 2_655 ?
Cl1 Ti1 Cl2 90.11(5) 2_655 . ?
Cl1 Ti1 Cl2 89.89(5) . . ?
Cl1 Ti1 Cl2 89.89(5) 2_655 2_655 ?
Cl2 Ti1 Cl2 180.0 2_655 . ?
O005 Ti1 Cl1 90.19(11) 2_655 2_655 ?
O005 Ti1 Cl1 89.81(11) . 2_655 ?
O005 Ti1 Cl1 89.81(11) 2_655 . ?
O005 Ti1 Cl1 90.19(11) . . ?
O005 Ti1 Cl2 89.98(11) 2_655 2_655 ?
O005 Ti1 Cl2 89.98(11) . . ?
O005 Ti1 Cl2 90.02(11) 2_655 . ?
O005 Ti1 Cl2 90.02(11) . 2_655 ?
O005 Ti1 O005 180.0 2_655 . ?
O005 P1 C13 107.8(2) . . ?
O005 P1 C1 111.7(2) . . ?
O005 P1 C7 110.9(2) . . ?
C13 P1 C1 109.4(3) . . ?
C13 P1 C7 109.3(3) . . ?
C7 P1 C1 107.8(3) . . ?
P1 O005 Ti1 162.3(2) . . ?
C14 C13 P1 118.2(5) . . ?
C18 C13 P1 121.9(4) . . ?
C18 C13 C14 120.0(5) . . ?
C2 C1 P1 118.6(4) . . ?
C6 C1 P1 121.8(4) . . ?
C6 C1 C2 119.5(5) . . ?
C8 C7 P1 118.7(5) . . ?
C8 C7 C12 120.4(6) . . ?
C12 C7 P1 120.8(5) . . ?
C1 C2 H2 119.9 . . ?
C3 C2 C1 120.3(6) . . ?
C3 C2 H2 119.9 . . ?
C7 C8 H8 120.4 . . ?
C7 C8 C9 119.3(6) . . ?
C9 C8 H8 120.4 . . ?
C1 C6 H6 120.2 . . ?
C1 C6 C5 119.5(6) . . ?
C5 C6 H6 120.2 . . ?
C7 C12 H12 120.7 . . ?
C11 C12 C7 118.7(6) . . ?
C11 C12 H12 120.7 . . ?
C13 C14 H14 120.0 . . ?
C13 C14 C15 120.0(6) . . ?
C15 C14 H14 120.0 . . ?
C12 C11 H11 120.1 . . ?
C10 C11 C12 119.9(6) . . ?
C10 C11 H11 120.1 . . ?
C2 C3 H3 119.7 . . ?
C2 C3 C4 120.5(6) . . ?
C4 C3 H3 119.7 . . ?
C13 C18 H18 120.0 . . ?
C13 C18 C17 120.1(6) . . ?
C17 C18 H18 120.0 . . ?
C11 C10 H10 119.2 . . ?
C9 C10 C11 121.7(6) . . ?
C9 C10 H10 119.2 . . ?
C3 C4 H4 119.9 . . ?
C5 C4 C3 120.2(6) . . ?
C5 C4 H4 119.9 . . ?
C6 C5 H5 120.1 . . ?
C4 C5 C6 119.9(6) . . ?
C4 C5 H5 120.1 . . ?
C8 C9 H9 120.0 . . ?
C10 C9 C8 119.9(7) . . ?
C10 C9 H9 120.0 . . ?
C18 C17 H17 121.0 . . ?
C16 C17 C18 118.1(6) . . ?
C16 C17 H17 121.0 . . ?
C14 C15 H15 120.1 . . ?
C16 C15 C14 119.9(6) . . ?
C16 C15 H15 120.1 . . ?
C17 C16 H16 119.0 . . ?
C15 C16 C17 122.0(6) . . ?
C15 C16 H16 119.0 . . ?

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
P1 C13 C14 C15 -178.2(5) . . . . ?
P1 C13 C18 C17 177.1(5) . . . . ?
P1 C1 C2 C3 -177.9(5) . . . . ?
P1 C1 C6 C5 175.7(5) . . . . ?
P1 C7 C8 C9 -175.5(5) . . . . ?
P1 C7 C12 C11 176.0(4) . . . . ?
O005 P1 C13 C14 -40.9(5) . . . . ?
O005 P1 C13 C18 140.2(5) . . . . ?
O005 P1 C1 C2 -56.7(5) . . . . ?
O005 P1 C1 C6 125.6(5) . . . . ?
O005 P1 C7 C8 -35.9(5) . . . . ?
O005 P1 C7 C12 145.9(5) . . . . ?
C13 P1 O005 Ti1 174.2(8) . . . . ?
C13 P1 C1 C2 -175.9(4) . . . . ?
C13 P1 C1 C6 6.3(6) . . . . ?
C13 P1 C7 C8 82.8(5) . . . . ?
C13 P1 C7 C12 -95.4(5) . . . . ?
C13 C14 C15 C16 1.2(10) . . . . ?
C13 C18 C17 C16 0.9(10) . . . . ?
C1 P1 O005 Ti1 54.0(8) . . . . ?
C1 P1 C13 C14 80.7(5) . . . . ?
C1 P1 C13 C18 -98.2(5) . . . . ?
C1 P1 C7 C8 -158.4(5) . . . . ?
C1 P1 C7 C12 23.4(5) . . . . ?
C1 C2 C3 C4 1.7(10) . . . . ?
C1 C6 C5 C4 2.5(10) . . . . ?
C7 P1 O005 Ti1 -66.2(8) . . . . ?
C7 P1 C13 C14 -161.5(5) . . . . ?
C7 P1 C13 C18 19.6(6) . . . . ?
C7 P1 C1 C2 65.4(5) . . . . ?
C7 P1 C1 C6 -112.4(5) . . . . ?
C7 C8 C9 C10 -0.2(9) . . . . ?
C7 C12 C11 C10 -0.9(9) . . . . ?
C2 C1 C6 C5 -2.0(9) . . . . ?
C2 C3 C4 C5 -1.2(11) . . . . ?
C8 C7 C12 C11 -2.2(9) . . . . ?
C6 C1 C2 C3 -0.1(9) . . . . ?
C12 C7 C8 C9 2.7(9) . . . . ?
C12 C11 C10 C9 3.4(10) . . . . ?
C14 C13 C18 C17 -1.8(10) . . . . ?
C14 C15 C16 C17 -2.2(11) . . . . ?
C11 C10 C9 C8 -2.9(10) . . . . ?
C3 C4 C5 C6 -0.9(11) . . . . ?
C18 C13 C14 C15 0.8(9) . . . . ?
C18 C17 C16 C15 1.1(11) . . . . ?


_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_original_sample_id CS148
_olex2_submission_special_instructions 'No special instructions were received'
_STOE_detector_distance          '40.0 mm'
_STOE_detector_pixelsize_x       '0.075 mm'
_STOE_detector_pixelsize_y       '0.075 mm'
_STOE_detector_size_x            '8.0 cm'
_STOE_detector_size_y            '7.7 cm'
_STOE_evaluation_integration_A   5.6
_STOE_evaluation_integration_B   -1.0
_STOE_evaluation_integration_EMS 0.017
_STOE_evaluation_LANA_BIS_l_even_max -
_STOE_evaluation_LANA_BIS_l_odd_max -
_STOE_evaluation_LANA_BOS_l_even_max 4
_STOE_evaluation_LANA_BOS_l_odd_max 1
_STOE_evaluation_LANA_completeness 98.4
_STOE_evaluation_LANA_DXS_max_order 1
_STOE_evaluation_LANA_DYS_max_order 1
_STOE_evaluation_LANA_FS_max_order 3
_STOE_evaluation_LANA_max_2theta_available 145.8
_STOE_evaluation_LANA_max_2theta_desired 145.8
_STOE_evaluation_LANA_mean_redundancy 4.5
_STOE_evaluation_LANA_number_refls_after_OR 15136
_STOE_evaluation_LANA_number_refls_outliers 6338
_STOE_evaluation_LANA_number_refls_total 21474
_STOE_evaluation_LANA_number_refls_unique 3387
_STOE_evaluation_LANA_number_refls_written 15136
_STOE_evaluation_LANA_OR_c1      0.035
_STOE_evaluation_LANA_OR_c2      0
_STOE_evaluation_LANA_OR_c3      0
_STOE_evaluation_LANA_OR_c4      0.7
_STOE_evaluation_LANA_point_group -1
_STOE_evaluation_LANA_table      
;
#----------------------------------------------------------------------------
2Theta          15.9   31.3   46.7   62.1   77.5   92.9  108.3  123.7  139.1
#----------------------------------------------------------------------------
<Resolution>    4.71   2.70   1.92   1.46   1.23   1.07   0.95   0.87   0.83
N(total)          69    344    816   2617   4503   4532   3306   3483   1804
<Redundancy>     1.7    2.2    2.5    5.1    6.6    5.5    3.9    4.2    3.1
Complet. [%%]    97.3   99.1  100.0  100.0  100.0   99.7   99.2   98.6   91.9
<I/sigma>      283.9  139.1   83.9   46.6   33.8   27.5   19.7   11.7    6.5
R(int)         0.051  0.034  0.038  0.042  0.043  0.046  0.078  0.161  0.247
#----------------------------------------------------------------------------
;
_STOE_measurement_identifier     CS148_150K
_STOE_measurement_max_exposure_per_frame '10.0 s'
_STOE_measurement_mean_exposure_per_frame '9.7 s'
_STOE_measurement_min_exposure_per_frame '2.0 s'
_STOE_measurement_total_exposure_time '9.9 h'
_STOE_measurement_total_frame_number 3675
_STOE_measurement_total_run_number 34
_STOE_measurement_tube_power     '50.0 W'
####################################################################### 
# 
# 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_por195_150k
_audit_block_doi                 10.5517/ccdc.csd.cc2dhp6t
_database_code_depnum_ccdc_archive 'CCDC 2219606'
loop_
_citation_id
_citation_doi
_citation_year
1 10.26434/chemrxiv-2023-rcvdn 2023
loop_
_audit_author_name
_audit_author_address
'Alessandro Prescimone'
;University Basel
Switzerland
;
_audit_update_record             
;
2022-11-14 deposited with the CCDC.	2024-05-06 downloaded from the CCDC.
;
_audit_creation_date             2022-10-03
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
rohan.pokratath@unibas.ch
alessandro.prescimone@unibas.ch
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C8 H16 Br4 O2 Zr'
_chemical_formula_sum            'C8 H16 Br4 O2 Zr'
_chemical_formula_weight         555.07
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -0.1862 2.2449 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.1420(7)
_cell_length_b                   7.5304(8)
_cell_length_c                   8.0799(8)
_cell_angle_alpha                87.085(8)
_cell_angle_beta                 68.311(8)
_cell_angle_gamma                71.788(8)
_cell_volume                     382.53(7)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    7773
_cell_measurement_temperature    150
_cell_measurement_theta_max      71.50
_cell_measurement_theta_min      5.91
_shelx_estimated_absorpt_T_max   0.366
_shelx_estimated_absorpt_T_min   0.089
_exptl_absorpt_coefficient_mu    17.995
_exptl_absorpt_correction_T_max  0.0000
_exptl_absorpt_correction_T_min  0.0000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens in: F. R. Ahmed (Editor), "Crystallographic Computing", Munksgaard,
Copenhagen (1970), 255 - 270. Afterwards scaling of reflection intensities was
performed within STOE LANA. J. Koziskova, F. Hahn, J. Richter, J. Kozisek, Acta
Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Finally a spherical absorption correction was done within STOE LANA.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.410
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             260
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-3 -1 30 0.0191
-6 -30 -29 0.0521
30 17 -7 0.0534
-13 26 30 0.0524
-24 5 -30 0.0649
12 23 30 0.0510
-1 0 -15 0.0264
-14 -5 15 0.0515
11 -27 -30 0.0534

_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.183
_exptl_crystal_size_min          0.07
_exptl_crystal_size_rad          0.180
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0482
_diffrn_reflns_av_unetI/netI     0.0283
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            6412
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         73.062
_diffrn_reflns_theta_min         7.312
_diffrn_ambient_temperature      150
_diffrn_detector                 'EIGER2 1M'
_diffrn_detector_area_resol_mean 13.33
_diffrn_detector_type            ?
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_details      
;
 3719 frames, detector distance = 40 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, ω scans'
_diffrn_radiation_collimation    '1.2 0.6 mm diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  270
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54186
_diffrn_source                   'Axo Cu'
_diffrn_source_current           1.00
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1079
_reflns_number_total             1496
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'X-Area Recipe 1.37.0.0 (STOE, 2021)'
_computing_data_collection       'X-Area Pilatus3_SV 1.31.186.0 (STOE, 2022)'
_computing_data_reduction        
;
X-Area Integrate 2.5.3.0 (STOE, 2021)
X-Area LANA 2.7.5.0 (STOE, 2022)
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.089
_refine_diff_density_min         -0.914
_refine_diff_density_rms         0.204
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     70
_refine_ls_number_reflns         1496
_refine_ls_number_restraints     60
_refine_ls_R_factor_all          0.1156
_refine_ls_R_factor_gt           0.0846
_refine_ls_restrained_S_all      1.079
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0400P)²+4.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1752
_refine_ls_wR_factor_ref         0.1949
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
O1 \\sim C4 \\sim C3 \\sim C2 \\sim C1: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
3. Rigid body (RIGU) restrains
 C1, C2, C3, C4, O1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C2(H2A,H2B), C4(H4A,H4B), C1(H1A,H1B)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zr1 Zr 0.500000 0.500000 0.500000 0.0998(6) Uani 1 2 d S . P . .
Br1 Br 0.5829(3) 0.6165(3) 0.7520(2) 0.1128(7) Uani 1 1 d . . . . .
Br2 Br 0.1502(3) 0.7765(2) 0.5865(2) 0.1109(6) Uani 1 1 d . . . . .
O1 O 0.3372(16) 0.3264(14) 0.6837(13) 0.104(3) Uani 1 1 d . U . . .
C3 C 0.234(3) 0.135(2) 0.917(2) 0.123(5) Uani 1 1 d . U . . .
H3A H 0.277996 -0.001670 0.890249 0.147 Uiso 1 1 calc R U . . .
H3B H 0.196805 0.159690 1.046715 0.147 Uiso 1 1 calc R U . . .
C2 C 0.054(3) 0.230(3) 0.868(3) 0.126(5) Uani 1 1 d . U . . .
H2A H -0.044903 0.337015 0.955646 0.151 Uiso 1 1 calc R U . . .
H2B H -0.022897 0.143071 0.863987 0.151 Uiso 1 1 calc R U . . .
C4 C 0.411(3) 0.211(3) 0.810(2) 0.120(5) Uani 1 1 d . U . . .
H4A H 0.440228 0.286738 0.888519 0.144 Uiso 1 1 calc R U . . .
H4B H 0.542442 0.107504 0.746765 0.144 Uiso 1 1 calc R U . . .
C1 C 0.142(3) 0.298(3) 0.688(3) 0.122(5) Uani 1 1 d . U . . .
H1A H 0.172842 0.203802 0.592997 0.147 Uiso 1 1 calc R U . . .
H1B H 0.041475 0.416983 0.673981 0.147 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Zr1 Br1 2.5816(18) . ?
Zr1 Br1 2.5816(18) 2_666 ?
Zr1 Br2 2.5830(17) 2_666 ?
Zr1 Br2 2.5830(17) . ?
Zr1 O1 2.178(10) 2_666 ?
Zr1 O1 2.178(10) . ?
O1 C4 1.447(17) . ?
O1 C1 1.461(18) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C2 1.45(2) . ?
C3 C4 1.50(2) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C1 1.49(2) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?

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
Br1 Zr1 Br1 180.0 . 2_666 ?
Br1 Zr1 Br2 89.92(6) . 2_666 ?
Br1 Zr1 Br2 90.08(6) 2_666 2_666 ?
Br1 Zr1 Br2 89.92(6) 2_666 . ?
Br1 Zr1 Br2 90.08(6) . . ?
Br2 Zr1 Br2 180.0 . 2_666 ?
O1 Zr1 Br1 89.9(3) 2_666 2_666 ?
O1 Zr1 Br1 90.1(3) 2_666 . ?
O1 Zr1 Br1 89.9(3) . . ?
O1 Zr1 Br1 90.1(3) . 2_666 ?
O1 Zr1 Br2 90.8(3) . . ?
O1 Zr1 Br2 89.2(3) 2_666 . ?
O1 Zr1 Br2 89.2(3) . 2_666 ?
O1 Zr1 Br2 90.8(3) 2_666 2_666 ?
O1 Zr1 O1 180.0 . 2_666 ?
C4 O1 Zr1 126.1(9) . . ?
C4 O1 C1 109.3(12) . . ?
C1 O1 Zr1 124.5(9) . . ?
H3A C3 H3B 108.6 . . ?
C2 C3 H3A 110.4 . . ?
C2 C3 H3B 110.4 . . ?
C2 C3 C4 106.8(14) . . ?
C4 C3 H3A 110.4 . . ?
C4 C3 H3B 110.4 . . ?
C3 C2 H2A 110.4 . . ?
C3 C2 H2B 110.4 . . ?
C3 C2 C1 106.4(15) . . ?
H2A C2 H2B 108.6 . . ?
C1 C2 H2A 110.4 . . ?
C1 C2 H2B 110.4 . . ?
O1 C4 C3 105.7(14) . . ?
O1 C4 H4A 110.6 . . ?
O1 C4 H4B 110.6 . . ?
C3 C4 H4A 110.6 . . ?
C3 C4 H4B 110.6 . . ?
H4A C4 H4B 108.7 . . ?
O1 C1 C2 104.0(14) . . ?
O1 C1 H1A 111.0 . . ?
O1 C1 H1B 111.0 . . ?
C2 C1 H1A 111.0 . . ?
C2 C1 H1B 111.0 . . ?
H1A C1 H1B 109.0 . . ?

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
Zr1 O1 C4 C3 174.4(10) . . . . ?
Zr1 O1 C1 C2 -160.7(10) . . . . ?
C3 C2 C1 O1 -28.2(19) . . . . ?
C2 C3 C4 O1 -8(2) . . . . ?
C4 O1 C1 C2 23.4(18) . . . . ?
C4 C3 C2 C1 23(2) . . . . ?
C1 O1 C4 C3 -9.7(19) . . . . ?


_olex2_date_sample_data_collection 2022-09-30
_olex2_date_sample_submission    2022-09-16
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a mylar loop in perfluoroether oil'
_olex2_submission_original_sample_id POR195_150K
_olex2_submission_special_instructions 'No special instructions were received'
_STOE_detector_distance          '40.0 mm'
_STOE_detector_pixelsize_x       '0.075 mm'
_STOE_detector_pixelsize_y       '0.075 mm'
_STOE_detector_size_x            '8.0 cm'
_STOE_detector_size_y            '7.7 cm'
_STOE_evaluation_integration_A   5.6
_STOE_evaluation_integration_B   -1.0
_STOE_evaluation_integration_EMS 0.017
_STOE_evaluation_LANA_BIS_l_even_max -
_STOE_evaluation_LANA_BIS_l_odd_max -
_STOE_evaluation_LANA_BOS_l_even_max 6
_STOE_evaluation_LANA_BOS_l_odd_max 3
_STOE_evaluation_LANA_completeness 98.2
_STOE_evaluation_LANA_DXS_max_order 1
_STOE_evaluation_LANA_DYS_max_order 1
_STOE_evaluation_LANA_FS_max_order 3
_STOE_evaluation_LANA_max_2theta_available 146.2
_STOE_evaluation_LANA_max_2theta_desired 146.2
_STOE_evaluation_LANA_mean_redundancy 4.3
_STOE_evaluation_LANA_number_refls_after_OR 6422
_STOE_evaluation_LANA_number_refls_outliers 2741
_STOE_evaluation_LANA_number_refls_total 9163
_STOE_evaluation_LANA_number_refls_unique 1501
_STOE_evaluation_LANA_number_refls_written 6422
_STOE_evaluation_LANA_OR_c1      0.035
_STOE_evaluation_LANA_OR_c2      0
_STOE_evaluation_LANA_OR_c3      0
_STOE_evaluation_LANA_OR_c4      0.7
_STOE_evaluation_LANA_point_group -1
_STOE_evaluation_LANA_table      
;
#----------------------------------------------------------------------------
2Theta          19.3   34.3   49.3   64.3   79.3   94.3  109.3  124.3  139.3
#----------------------------------------------------------------------------
<Resolution>    4.14   2.55   1.83   1.42   1.21   1.06   0.94   0.87   0.83
N(total)          59    231    412   1289   1814   1743   1426   1401    788
<Redundancy>     2.2    2.8    2.4    5.2    5.8    4.7    4.1    4.1    3.4
Complet. [%%]   100.0  100.0  100.0  100.0   99.5   99.6   99.2   98.4   90.4
<I/sigma>      197.8  125.4   86.0   31.5   25.9   15.7    7.7    2.6    0.8
R(int)         0.035  0.028  0.030  0.072  0.065  0.088  0.153  0.366  0.481
#----------------------------------------------------------------------------
;
_STOE_measurement_identifier     POR195_150K
_STOE_measurement_max_exposure_per_frame '2.0 s'
_STOE_measurement_mean_exposure_per_frame '1.9 s'
_STOE_measurement_min_exposure_per_frame '1.0 s'
_STOE_measurement_total_exposure_time '2.0 h'
_STOE_measurement_total_frame_number 3719
_STOE_measurement_total_run_number 33
_STOE_measurement_tube_power     '50.0 W'
####################################################################### 
# 
# 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_cs145_150k
_audit_block_doi                 10.5517/ccdc.csd.cc2dhp1n
_database_code_depnum_ccdc_archive 'CCDC 2219601'
loop_
_citation_id
_citation_doi
_citation_year
1 10.26434/chemrxiv-2023-rcvdn 2023
_audit_update_record             
;
2024-01-23 deposited with the CCDC.	2024-05-06 downloaded from the CCDC.
;
_audit_creation_date             2023-11-14
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
alessandro.prescimone@unibas.ch
carlotta.seno@unibas.ch
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C36 H30 Cl4 O2 P2 Zr'
_chemical_formula_sum            'C36 H30 Cl4 O2 P2 Zr'
_chemical_formula_weight         789.56
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -0.1862 2.2449 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.4661(4)
_cell_length_b                   9.5612(4)
_cell_length_c                   10.5356(4)
_cell_angle_alpha                101.126(3)
_cell_angle_beta                 107.899(3)
_cell_angle_gamma                92.429(3)
_cell_volume                     885.05(6)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    34110
_cell_measurement_temperature    150
_cell_measurement_theta_max      73.15
_cell_measurement_theta_min      4.52
_shelx_estimated_absorpt_T_max   0.446
_shelx_estimated_absorpt_T_min   0.408
_exptl_absorpt_coefficient_mu    6.427
_exptl_absorpt_correction_T_max  0.0017
_exptl_absorpt_correction_T_min  0.0003
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens in: F. R. Ahmed (Editor), "Crystallographic Computing", Munksgaard,
Copenhagen (1970), 255 - 270. Afterwards scaling of reflection intensities was
performed within STOE LANA. J. Koziskova, F. Hahn, J. Richter, J. Kozisek, Acta
Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Finally a spherical absorption correction was done within STOE LANA.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.481
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             400
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 1 30 0.0672
-4 -19 -30 0.0446
-14 15 13 0.0459
-4 -15 4 0.0648
-30 1 -21 0.0674
9 30 22 0.0526
1 -1 -15 0.0556
29 13 30 0.0531
-2 15 -9 0.0943
-29 -30 5 0.0848
18 -30 -25 0.0592

_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.157
_exptl_crystal_size_min          0.15
_exptl_crystal_size_rad          0.150
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0353
_diffrn_reflns_av_unetI/netI     0.0203
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            16749
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         72.804
_diffrn_reflns_theta_min         4.518
_diffrn_ambient_temperature      150
_diffrn_detector                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 300K'
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_details      
;
 4262 frames, detector distance = 40 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, ω scans'
_diffrn_radiation_collimation    '1.2 0.6 mm diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  270
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.54186
_diffrn_source                   'Axo Cu'
_diffrn_source_current           3.570
_diffrn_source_power             0.250
_diffrn_source_voltage           70
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3120
_reflns_number_total             3432
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'X-Area Recipe 1.37.0.0 (STOE, 2021)'
_computing_data_collection       'X-Area Pilatus3_SV 1.31.175.0 (STOE, 2021)'
_computing_data_reduction        
;
X-Area Integrate 2.5.1.0 (STOE, 2021)
X-Area LANA 2.6.2.0 (STOE, 2021)
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         1.145
_refine_diff_density_min         -1.273
_refine_diff_density_rms         0.148
_refine_ls_extinction_coef       0.0187(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   0.903
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     206
_refine_ls_number_reflns         3432
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0979
_refine_ls_R_factor_gt           0.0840
_refine_ls_restrained_S_all      0.903
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0400P)²+9.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1668
_refine_ls_wR_factor_ref         0.1820
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C14(H14), C2(H2), C6(H6), C5(H5), C16(H16), C8(H8), C17(H17), C3(H3),
 C11(H11), C12(H12), C9(H9), C15(H15), C18(H18), C10(H10)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zr1 Zr 0.000000 0.000000 0.000000 0.0540(3) Uani 1 2 d S . P . .
Cl2 Cl -0.1456(2) -0.0498(2) 0.1465(2) 0.0647(5) Uani 1 1 d . . . . .
Cl1 Cl -0.1828(2) 0.1562(2) -0.0969(2) 0.0637(5) Uani 1 1 d . . . . .
P1 P 0.2395(2) 0.2762(2) 0.2627(2) 0.0565(5) Uani 1 1 d . . . . .
O1 O 0.1198(5) 0.1730(5) 0.1504(5) 0.0595(12) Uani 1 1 d . . . . .
C1 C 0.3920(9) 0.3182(8) 0.2052(8) 0.0604(17) Uani 1 1 d . . . . .
C13 C 0.1600(8) 0.4358(8) 0.3106(8) 0.0607(18) Uani 1 1 d . . . . .
C4 C 0.6348(10) 0.3727(10) 0.1233(10) 0.080(2) Uani 1 1 d . . . . .
H4 H 0.719218 0.391596 0.096088 0.095 Uiso 1 1 calc R U . . .
C14 C 0.1975(9) 0.5108(9) 0.4458(9) 0.069(2) Uani 1 1 d . . . . .
H14 H 0.265165 0.475592 0.516606 0.083 Uiso 1 1 calc R U . . .
C2 C 0.4468(9) 0.4580(9) 0.2170(9) 0.071(2) Uani 1 1 d . . . . .
H2 H 0.401026 0.535362 0.253526 0.085 Uiso 1 1 calc R U . . .
C6 C 0.4582(9) 0.2059(9) 0.1511(9) 0.068(2) Uani 1 1 d . . . . .
H6 H 0.419768 0.109845 0.142156 0.081 Uiso 1 1 calc R U . . .
C7 C 0.3091(8) 0.1992(8) 0.4075(8) 0.0585(17) Uani 1 1 d . . . . .
C5 C 0.5799(9) 0.2326(10) 0.1099(9) 0.075(2) Uani 1 1 d . . . . .
H5 H 0.625414 0.155400 0.072739 0.090 Uiso 1 1 calc R U . . .
C16 C 0.0388(10) 0.6890(10) 0.3730(11) 0.081(3) Uani 1 1 d . . . . .
H16 H -0.001554 0.776406 0.394219 0.097 Uiso 1 1 calc R U . . .
C8 C 0.4572(9) 0.2273(9) 0.4888(9) 0.069(2) Uani 1 1 d . . . . .
H8 H 0.525570 0.283673 0.464221 0.083 Uiso 1 1 calc R U . . .
C17 C 0.0007(10) 0.6153(9) 0.2400(10) 0.077(2) Uani 1 1 d . . . . .
H17 H -0.066722 0.651363 0.169603 0.092 Uiso 1 1 calc R U . . .
C3 C 0.5688(10) 0.4849(10) 0.1754(10) 0.079(2) Uani 1 1 d . . . . .
H3 H 0.606659 0.580839 0.182991 0.095 Uiso 1 1 calc R U . . .
C11 C 0.2606(11) 0.0633(10) 0.5635(9) 0.076(2) Uani 1 1 d . . . . .
H11 H 0.193382 0.006151 0.588537 0.092 Uiso 1 1 calc R U . . .
C12 C 0.2099(10) 0.1157(9) 0.4436(8) 0.068(2) Uani 1 1 d . . . . .
H12 H 0.108437 0.094191 0.387334 0.082 Uiso 1 1 calc R U . . .
C9 C 0.5063(11) 0.1730(9) 0.6068(9) 0.075(2) Uani 1 1 d . . . . .
H9 H 0.608615 0.190059 0.661225 0.090 Uiso 1 1 calc R U . . .
C15 C 0.1359(10) 0.6368(9) 0.4768(10) 0.079(2) Uani 1 1 d . . . . .
H15 H 0.160218 0.687264 0.569093 0.095 Uiso 1 1 calc R U . . .
C18 C 0.0600(9) 0.4882(9) 0.2076(9) 0.067(2) Uani 1 1 d . . . . .
H18 H 0.032547 0.436961 0.115349 0.081 Uiso 1 1 calc R U . . .
C10 C 0.4063(12) 0.0945(9) 0.6443(9) 0.079(3) Uani 1 1 d . . . . .
H10 H 0.439087 0.061796 0.727141 0.094 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Zr1 Cl2 2.4583(18) 2 ?
Zr1 Cl2 2.4583(18) . ?
Zr1 Cl1 2.4477(17) . ?
Zr1 Cl1 2.4478(17) 2 ?
Zr1 O1 2.063(5) 2 ?
Zr1 O1 2.063(5) . ?
P1 O1 1.513(5) . ?
P1 C1 1.787(8) . ?
P1 C13 1.784(8) . ?
P1 C7 1.778(7) . ?
C1 C2 1.381(11) . ?
C1 C6 1.383(10) . ?
C13 C14 1.393(11) . ?
C13 C18 1.394(10) . ?
C4 H4 0.9500 . ?
C4 C5 1.381(12) . ?
C4 C3 1.372(12) . ?
C14 H14 0.9500 . ?
C14 C15 1.387(11) . ?
C2 H2 0.9500 . ?
C2 C3 1.386(11) . ?
C6 H6 0.9500 . ?
C6 C5 1.380(11) . ?
C7 C8 1.383(11) . ?
C7 C12 1.392(11) . ?
C5 H5 0.9500 . ?
C16 H16 0.9500 . ?
C16 C17 1.370(13) . ?
C16 C15 1.386(13) . ?
C8 H8 0.9500 . ?
C8 C9 1.395(11) . ?
C17 H17 0.9500 . ?
C17 C18 1.387(11) . ?
C3 H3 0.9500 . ?
C11 H11 0.9500 . ?
C11 C12 1.403(11) . ?
C11 C10 1.364(13) . ?
C12 H12 0.9500 . ?
C9 H9 0.9500 . ?
C9 C10 1.379(13) . ?
C15 H15 0.9500 . ?
C18 H18 0.9500 . ?
C10 H10 0.9500 . ?

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
Cl2 Zr1 Cl2 180.0 2 . ?
Cl1 Zr1 Cl2 89.99(6) 2 . ?
Cl1 Zr1 Cl2 90.01(6) . . ?
Cl1 Zr1 Cl2 89.99(6) . 2 ?
Cl1 Zr1 Cl2 90.01(6) 2 2 ?
Cl1 Zr1 Cl1 180.0 . 2 ?
O1 Zr1 Cl2 90.00(15) 2 2 ?
O1 Zr1 Cl2 90.00(15) 2 . ?
O1 Zr1 Cl2 90.00(15) . . ?
O1 Zr1 Cl2 90.00(15) . 2 ?
O1 Zr1 Cl1 90.08(14) 2 . ?
O1 Zr1 Cl1 89.92(14) 2 2 ?
O1 Zr1 Cl1 90.08(14) . 2 ?
O1 Zr1 Cl1 89.92(14) . . ?
O1 Zr1 O1 180.0 2 . ?
O1 P1 C1 110.4(3) . . ?
O1 P1 C13 108.6(3) . . ?
O1 P1 C7 110.5(3) . . ?
C13 P1 C1 109.9(3) . . ?
C7 P1 C1 108.2(3) . . ?
C7 P1 C13 109.2(4) . . ?
P1 O1 Zr1 165.5(3) . . ?
C2 C1 P1 122.0(6) . . ?
C6 C1 P1 118.1(6) . . ?
C6 C1 C2 119.9(8) . . ?
C14 C13 P1 122.4(6) . . ?
C18 C13 P1 118.1(6) . . ?
C18 C13 C14 119.5(7) . . ?
C5 C4 H4 119.6 . . ?
C3 C4 H4 119.6 . . ?
C3 C4 C5 120.8(8) . . ?
C13 C14 H14 120.0 . . ?
C15 C14 C13 120.0(8) . . ?
C15 C14 H14 120.0 . . ?
C1 C2 H2 120.1 . . ?
C1 C2 C3 119.7(8) . . ?
C3 C2 H2 120.1 . . ?
C1 C6 H6 119.8 . . ?
C5 C6 C1 120.4(8) . . ?
C5 C6 H6 119.8 . . ?
C8 C7 P1 121.4(6) . . ?
C8 C7 C12 119.7(7) . . ?
C12 C7 P1 118.9(6) . . ?
C4 C5 C6 119.3(8) . . ?
C4 C5 H5 120.4 . . ?
C6 C5 H5 120.4 . . ?
C17 C16 H16 119.8 . . ?
C17 C16 C15 120.5(8) . . ?
C15 C16 H16 119.8 . . ?
C7 C8 H8 120.0 . . ?
C7 C8 C9 120.0(8) . . ?
C9 C8 H8 120.0 . . ?
C16 C17 H17 119.9 . . ?
C16 C17 C18 120.3(8) . . ?
C18 C17 H17 119.9 . . ?
C4 C3 C2 119.9(8) . . ?
C4 C3 H3 120.1 . . ?
C2 C3 H3 120.1 . . ?
C12 C11 H11 119.9 . . ?
C10 C11 H11 119.9 . . ?
C10 C11 C12 120.1(9) . . ?
C7 C12 C11 119.6(8) . . ?
C7 C12 H12 120.2 . . ?
C11 C12 H12 120.2 . . ?
C8 C9 H9 120.0 . . ?
C10 C9 C8 120.0(8) . . ?
C10 C9 H9 120.0 . . ?
C14 C15 H15 120.1 . . ?
C16 C15 C14 119.8(9) . . ?
C16 C15 H15 120.1 . . ?
C13 C18 H18 120.1 . . ?
C17 C18 C13 119.9(8) . . ?
C17 C18 H18 120.1 . . ?
C11 C10 C9 120.6(8) . . ?
C11 C10 H10 119.7 . . ?
C9 C10 H10 119.7 . . ?

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
P1 C1 C2 C3 177.6(7) . . . . ?
P1 C1 C6 C5 -177.6(7) . . . . ?
P1 C13 C14 C15 178.0(6) . . . . ?
P1 C13 C18 C17 -177.3(6) . . . . ?
P1 C7 C8 C9 175.8(6) . . . . ?
P1 C7 C12 C11 -175.0(6) . . . . ?
O1 P1 C1 C2 127.9(7) . . . . ?
O1 P1 C1 C6 -53.9(7) . . . . ?
O1 P1 C13 C14 141.8(6) . . . . ?
O1 P1 C13 C18 -40.0(7) . . . . ?
O1 P1 C7 C8 145.7(6) . . . . ?
O1 P1 C7 C12 -38.0(7) . . . . ?
C1 P1 O1 Zr1 58.9(13) . . . . ?
C1 P1 C13 C14 -97.3(7) . . . . ?
C1 P1 C13 C18 80.9(7) . . . . ?
C1 P1 C7 C8 24.7(8) . . . . ?
C1 P1 C7 C12 -159.1(6) . . . . ?
C1 C2 C3 C4 -0.3(14) . . . . ?
C1 C6 C5 C4 0.0(13) . . . . ?
C13 P1 O1 Zr1 179.4(12) . . . . ?
C13 P1 C1 C2 8.1(8) . . . . ?
C13 P1 C1 C6 -173.8(6) . . . . ?
C13 P1 C7 C8 -94.9(7) . . . . ?
C13 P1 C7 C12 81.4(7) . . . . ?
C13 C14 C15 C16 -0.9(13) . . . . ?
C14 C13 C18 C17 1.0(12) . . . . ?
C2 C1 C6 C5 0.6(13) . . . . ?
C6 C1 C2 C3 -0.5(13) . . . . ?
C7 P1 O1 Zr1 -60.8(14) . . . . ?
C7 P1 C1 C2 -111.0(7) . . . . ?
C7 P1 C1 C6 67.1(7) . . . . ?
C7 P1 C13 C14 21.2(8) . . . . ?
C7 P1 C13 C18 -160.5(6) . . . . ?
C7 C8 C9 C10 -1.8(13) . . . . ?
C5 C4 C3 C2 0.9(15) . . . . ?
C16 C17 C18 C13 -0.6(13) . . . . ?
C8 C7 C12 C11 1.3(12) . . . . ?
C8 C9 C10 C11 3.2(13) . . . . ?
C17 C16 C15 C14 1.4(14) . . . . ?
C3 C4 C5 C6 -0.7(15) . . . . ?
C12 C7 C8 C9 -0.5(12) . . . . ?
C12 C11 C10 C9 -2.4(13) . . . . ?
C15 C16 C17 C18 -0.6(14) . . . . ?
C18 C13 C14 C15 -0.3(12) . . . . ?
C10 C11 C12 C7 0.1(13) . . . . ?


_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'
_STOE_detector_distance          '40.0 mm'
_STOE_detector_pixelsize_x       '0.075 mm'
_STOE_detector_pixelsize_y       '0.075 mm'
_STOE_detector_size_x            '8.0 cm'
_STOE_detector_size_y            '7.7 cm'
_STOE_evaluation_integration_A   5.6
_STOE_evaluation_integration_B   -1.0
_STOE_evaluation_integration_EMS 0.017
_STOE_evaluation_LANA_BIS_l_even_max -
_STOE_evaluation_LANA_BIS_l_odd_max -
_STOE_evaluation_LANA_BOS_l_even_max 6
_STOE_evaluation_LANA_BOS_l_odd_max 3
_STOE_evaluation_LANA_completeness 97.4
_STOE_evaluation_LANA_DXS_max_order 1
_STOE_evaluation_LANA_DYS_max_order 1
_STOE_evaluation_LANA_FS_max_order 3
_STOE_evaluation_LANA_max_2theta_available 145.7
_STOE_evaluation_LANA_max_2theta_desired 145.7
_STOE_evaluation_LANA_mean_redundancy 4.9
_STOE_evaluation_LANA_number_refls_after_OR 16758
_STOE_evaluation_LANA_number_refls_outliers 7115
_STOE_evaluation_LANA_number_refls_total 23873
_STOE_evaluation_LANA_number_refls_unique 3437
_STOE_evaluation_LANA_number_refls_written 16758
_STOE_evaluation_LANA_OR_c1      0.035
_STOE_evaluation_LANA_OR_c2      0
_STOE_evaluation_LANA_OR_c3      0
_STOE_evaluation_LANA_OR_c4      0.7
_STOE_evaluation_LANA_point_group -1
_STOE_evaluation_LANA_table      
;
#----------------------------------------------------------------------------
2Theta          15.8   31.2   46.6   62.0   77.4   92.8  108.2  123.6  139.0
#----------------------------------------------------------------------------
<Resolution>    4.53   2.72   1.94   1.47   1.23   1.07   0.95   0.87   0.83
N(total)          98    611   1229   2855   5381   5010   3521   3303   1865
<Redundancy>     2.1    3.7    3.5    5.5    7.4    6.0    4.1    4.0    3.4
Complet. [%%]    97.4  100.0  100.0  100.0  100.0   99.7   99.5   97.3   85.5
<I/sigma>      247.0  120.3   89.2   47.8   34.2   29.9   21.2   12.3    6.0
R(int)         0.021  0.026  0.027  0.033  0.035  0.037  0.057  0.151  0.283
#----------------------------------------------------------------------------
;
_STOE_measurement_identifier     CS145_150K
_STOE_measurement_max_exposure_per_frame '8.0 s'
_STOE_measurement_mean_exposure_per_frame '6.3 s'
_STOE_measurement_min_exposure_per_frame '2.0 s'
_STOE_measurement_total_exposure_time '7.5 h'
_STOE_measurement_total_frame_number 4262
_STOE_measurement_total_run_number 71
_STOE_measurement_tube_power     '50.0 W'
####################################################################### 
# 
# 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_cs162_150k
_audit_block_doi                 10.5517/ccdc.csd.cc2dhp5s
_database_code_depnum_ccdc_archive 'CCDC 2219605'
loop_
_citation_id
_citation_doi
_citation_year
1 10.26434/chemrxiv-2023-rcvdn 2023
_audit_update_record             
;
2024-01-23 deposited with the CCDC.	2024-05-06 downloaded from the CCDC.
;
_audit_creation_date             2023-11-14
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
alessandro.prescimone@unibas.ch
carlotta.seno@unibas.ch
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C36 H30 Cl4 Hf O2 P2'
_chemical_formula_sum            'C36 H30 Cl4 Hf O2 P2'
_chemical_formula_weight         876.83
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Hf Hf -6.1794 4.9776 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.4917(3)
_cell_length_b                   9.5535(3)
_cell_length_c                   10.5075(3)
_cell_angle_alpha                101.253(2)
_cell_angle_beta                 108.000(2)
_cell_angle_gamma                92.173(3)
_cell_volume                     883.81(5)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    30074
_cell_measurement_temperature    150
_cell_measurement_theta_max      72.88
_cell_measurement_theta_min      4.54
_shelx_estimated_absorpt_T_max   0.426
_shelx_estimated_absorpt_T_min   0.284
_exptl_absorpt_coefficient_mu    9.344
_exptl_absorpt_correction_T_max  0.0002
_exptl_absorpt_correction_T_min  0.0000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens in: F. R. Ahmed (Editor), "Crystallographic Computing", Munksgaard,
Copenhagen (1970), 255 - 270. Afterwards scaling of reflection intensities was
performed within STOE LANA. J. Koziskova, F. Hahn, J. Richter, J. Kozisek, Acta
Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Finally a spherical absorption correction was done within STOE LANA.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.647
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             432
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
2 -3 30 0.0870
-17 -30 -21 0.0736
11 9 -15 0.0750
-29 26 30 0.1052
15 -30 17 0.0854
-30 2 -3 0.0990
3 15 1 0.0690
0 1 -5 0.0931
15 2 10 0.1049
1 28 -30 0.1010
-30 -6 25 0.0836
18 -30 -25 0.0928

_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.143
_exptl_crystal_size_min          0.11
_exptl_crystal_size_rad          0.140
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0253
_diffrn_reflns_av_unetI/netI     0.0157
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            14940
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         73.121
_diffrn_reflns_theta_min         4.746
_diffrn_ambient_temperature      150
_diffrn_detector                 'EIGER2 1M'
_diffrn_detector_area_resol_mean 13.33
_diffrn_detector_type            ?
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_details      
;
 3641 frames, detector distance = 40 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI Cu'
_diffrn_measurement_method       'rotation method, ω scans'
_diffrn_radiation_collimation    '1.2 0.6 mm diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  270
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54186
_diffrn_source                   'Axo Cu'
_diffrn_source_current           1.00
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3300
_reflns_number_total             3442
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'X-Area Recipe 1.37.0.0 (STOE, 2021)'
_computing_data_collection       'X-Area Pilatus3_SV 1.31.186.0 (STOE, 2022)'
_computing_data_reduction        
;
X-Area Integrate 2.5.3.0 (STOE, 2021)
X-Area LANA 2.7.5.0 (STOE, 2022)
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.203
_refine_diff_density_min         -1.421
_refine_diff_density_rms         0.144
_refine_ls_extinction_coef       0.0032(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     206
_refine_ls_number_reflns         3442
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0710
_refine_ls_R_factor_gt           0.0661
_refine_ls_restrained_S_all      1.036
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0600P)²+6.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1514
_refine_ls_wR_factor_ref         0.1588
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C8(H8), C14(H14), C15(H15), C12(H12), C2(H2), C6(H6), C5(H5), C16(H16),
 C18(H18), C10(H10), C9(H9), C11(H11), C4(H4), C3(H3), C17(H17)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Hf1 Hf 0.500000 1.000000 0.500000 0.0617(3) Uani 1 2 d S . P . .
Cl2 Cl 0.6824(2) 0.8448(2) 0.5971(2) 0.0712(5) Uani 1 1 d . . . . .
Cl1 Cl 0.3561(2) 0.9514(2) 0.6464(2) 0.0730(5) Uani 1 1 d . . . . .
P1 P 0.2615(2) 0.7243(2) 0.2378(2) 0.0661(5) Uani 1 1 d . . . . .
O1 O 0.3802(6) 0.8269(6) 0.3492(6) 0.0671(13) Uani 1 1 d . . . . .
C7 C 0.1913(10) 0.8007(9) 0.0917(9) 0.070(2) Uani 1 1 d . . . . .
C1 C 0.1098(10) 0.6827(10) 0.2957(9) 0.069(2) Uani 1 1 d . . . . .
C13 C 0.3404(10) 0.5634(9) 0.1902(9) 0.069(2) Uani 1 1 d . . . . .
C8 C 0.2907(12) 0.8844(10) 0.0557(10) 0.079(2) Uani 1 1 d . . . . .
H8 H 0.391879 0.906183 0.112302 0.095 Uiso 1 1 calc R U . . .
C14 C 0.4409(11) 0.5116(10) 0.2933(10) 0.076(2) Uani 1 1 d . . . . .
H14 H 0.468190 0.562636 0.386029 0.091 Uiso 1 1 calc R U . . .
C15 C 0.5006(12) 0.3860(11) 0.2602(13) 0.086(3) Uani 1 1 d . . . . .
H15 H 0.570023 0.350770 0.330180 0.103 Uiso 1 1 calc R U . . .
C12 C 0.0421(11) 0.7727(10) 0.0106(10) 0.077(2) Uani 1 1 d . . . . .
H12 H -0.025952 0.717424 0.035960 0.093 Uiso 1 1 calc R U . . .
C2 C 0.0555(11) 0.5425(11) 0.2847(10) 0.079(2) Uani 1 1 d . . . . .
H2 H 0.102573 0.464790 0.250249 0.095 Uiso 1 1 calc R U . . .
C6 C 0.0438(11) 0.7959(11) 0.3508(10) 0.079(2) Uani 1 1 d . . . . .
H6 H 0.082743 0.892101 0.361361 0.094 Uiso 1 1 calc R U . . .
C5 C -0.0789(11) 0.7684(11) 0.3902(11) 0.083(3) Uani 1 1 d . . . . .
H5 H -0.125380 0.845757 0.426021 0.099 Uiso 1 1 calc R U . . .
C16 C 0.4604(13) 0.3116(12) 0.1270(13) 0.091(3) Uani 1 1 d . . . . .
H16 H 0.500494 0.223731 0.105862 0.109 Uiso 1 1 calc R U . . .
C18 C 0.3037(11) 0.4897(11) 0.0554(10) 0.079(2) Uani 1 1 d . . . . .
H18 H 0.237714 0.526736 -0.015411 0.095 Uiso 1 1 calc R U . . .
C10 C 0.0928(14) 0.9040(11) -0.1452(10) 0.089(3) Uani 1 1 d . . . . .
H10 H 0.059657 0.936745 -0.228196 0.107 Uiso 1 1 calc R U . . .
C9 C 0.2399(13) 0.9352(12) -0.0636(10) 0.086(3) Uani 1 1 d . . . . .
H9 H 0.306691 0.991671 -0.089323 0.104 Uiso 1 1 calc R U . . .
C11 C -0.0062(13) 0.8260(11) -0.1074(10) 0.087(3) Uani 1 1 d . . . . .
H11 H -0.108186 0.808575 -0.162411 0.105 Uiso 1 1 calc R U . . .
C4 C -0.1338(12) 0.6289(13) 0.3776(12) 0.091(3) Uani 1 1 d . . . . .
H4 H -0.217242 0.610635 0.405985 0.109 Uiso 1 1 calc R U . . .
C3 C -0.0684(12) 0.5162(12) 0.3244(11) 0.089(3) Uani 1 1 d . . . . .
H3 H -0.107658 0.420309 0.314583 0.107 Uiso 1 1 calc R U . . .
C17 C 0.3627(13) 0.3620(11) 0.0228(12) 0.090(3) Uani 1 1 d . . . . .
H17 H 0.336260 0.310260 -0.069629 0.108 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Hf1 Cl2 2.4349(19) 2_676 ?
Hf1 Cl2 2.4349(19) . ?
Hf1 Cl1 2.445(2) 2_676 ?
Hf1 Cl1 2.445(2) . ?
Hf1 O1 2.064(5) . ?
Hf1 O1 2.064(5) 2_676 ?
P1 O1 1.502(6) . ?
P1 C7 1.782(9) . ?
P1 C1 1.787(9) . ?
P1 C13 1.787(9) . ?
C7 C8 1.398(13) . ?
C7 C12 1.392(12) . ?
C1 C2 1.387(13) . ?
C1 C6 1.389(12) . ?
C13 C14 1.391(12) . ?
C13 C18 1.382(13) . ?
C8 H8 0.9500 . ?
C8 C9 1.386(13) . ?
C14 H14 0.9500 . ?
C14 C15 1.375(13) . ?
C15 H15 0.9500 . ?
C15 C16 1.368(16) . ?
C12 H12 0.9500 . ?
C12 C11 1.386(13) . ?
C2 H2 0.9500 . ?
C2 C3 1.393(13) . ?
C6 H6 0.9500 . ?
C6 C5 1.383(13) . ?
C5 H5 0.9500 . ?
C5 C4 1.378(15) . ?
C16 H16 0.9500 . ?
C16 C17 1.379(15) . ?
C18 H18 0.9500 . ?
C18 C17 1.388(13) . ?
C10 H10 0.9500 . ?
C10 C9 1.379(15) . ?
C10 C11 1.375(16) . ?
C9 H9 0.9500 . ?
C11 H11 0.9500 . ?
C4 H4 0.9500 . ?
C4 C3 1.374(15) . ?
C3 H3 0.9500 . ?
C17 H17 0.9500 . ?

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
Cl2 Hf1 Cl2 180.0 2_676 . ?
Cl2 Hf1 Cl1 90.07(7) . . ?
Cl2 Hf1 Cl1 90.07(7) 2_676 2_676 ?
Cl2 Hf1 Cl1 89.93(7) . 2_676 ?
Cl2 Hf1 Cl1 89.93(7) 2_676 . ?
Cl1 Hf1 Cl1 180.0 . 2_676 ?
O1 Hf1 Cl2 90.12(16) 2_676 2_676 ?
O1 Hf1 Cl2 89.88(16) . 2_676 ?
O1 Hf1 Cl2 89.88(16) 2_676 . ?
O1 Hf1 Cl2 90.12(16) . . ?
O1 Hf1 Cl1 90.02(17) 2_676 . ?
O1 Hf1 Cl1 90.02(17) . 2_676 ?
O1 Hf1 Cl1 89.98(17) 2_676 2_676 ?
O1 Hf1 Cl1 89.98(17) . . ?
O1 Hf1 O1 180.0 2_676 . ?
O1 P1 C7 110.5(4) . . ?
O1 P1 C1 110.6(4) . . ?
O1 P1 C13 108.7(4) . . ?
C7 P1 C1 108.3(4) . . ?
C7 P1 C13 109.3(4) . . ?
C13 P1 C1 109.5(4) . . ?
P1 O1 Hf1 165.5(4) . . ?
C8 C7 P1 118.6(7) . . ?
C12 C7 P1 121.1(7) . . ?
C12 C7 C8 120.2(9) . . ?
C2 C1 P1 122.1(7) . . ?
C2 C1 C6 119.8(9) . . ?
C6 C1 P1 118.0(7) . . ?
C14 C13 P1 118.2(7) . . ?
C18 C13 P1 122.0(7) . . ?
C18 C13 C14 119.7(9) . . ?
C7 C8 H8 120.4 . . ?
C9 C8 C7 119.2(10) . . ?
C9 C8 H8 120.4 . . ?
C13 C14 H14 120.2 . . ?
C15 C14 C13 119.5(10) . . ?
C15 C14 H14 120.2 . . ?
C14 C15 H15 119.8 . . ?
C16 C15 C14 120.3(10) . . ?
C16 C15 H15 119.8 . . ?
C7 C12 H12 120.3 . . ?
C11 C12 C7 119.5(10) . . ?
C11 C12 H12 120.3 . . ?
C1 C2 H2 120.1 . . ?
C1 C2 C3 119.7(9) . . ?
C3 C2 H2 120.1 . . ?
C1 C6 H6 120.1 . . ?
C5 C6 C1 119.9(9) . . ?
C5 C6 H6 120.1 . . ?
C6 C5 H5 119.9 . . ?
C4 C5 C6 120.2(9) . . ?
C4 C5 H5 119.9 . . ?
C15 C16 H16 119.4 . . ?
C15 C16 C17 121.1(10) . . ?
C17 C16 H16 119.4 . . ?
C13 C18 H18 119.8 . . ?
C13 C18 C17 120.4(10) . . ?
C17 C18 H18 119.8 . . ?
C9 C10 H10 119.7 . . ?
C11 C10 H10 119.7 . . ?
C11 C10 C9 120.6(9) . . ?
C8 C9 H9 119.9 . . ?
C10 C9 C8 120.2(11) . . ?
C10 C9 H9 119.9 . . ?
C12 C11 H11 119.9 . . ?
C10 C11 C12 120.2(10) . . ?
C10 C11 H11 119.9 . . ?
C5 C4 H4 119.8 . . ?
C3 C4 C5 120.3(10) . . ?
C3 C4 H4 119.8 . . ?
C2 C3 H3 120.0 . . ?
C4 C3 C2 120.0(10) . . ?
C4 C3 H3 120.0 . . ?
C16 C17 C18 118.8(10) . . ?
C16 C17 H17 120.6 . . ?
C18 C17 H17 120.6 . . ?

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
P1 C7 C8 C9 175.0(7) . . . . ?
P1 C7 C12 C11 -175.6(7) . . . . ?
P1 C1 C2 C3 -176.4(8) . . . . ?
P1 C1 C6 C5 176.6(8) . . . . ?
P1 C13 C14 C15 178.4(7) . . . . ?
P1 C13 C18 C17 -177.4(8) . . . . ?
O1 P1 C7 C8 37.6(8) . . . . ?
O1 P1 C7 C12 -145.4(7) . . . . ?
O1 P1 C1 C2 -127.6(8) . . . . ?
O1 P1 C1 C6 53.6(8) . . . . ?
O1 P1 C13 C14 39.5(8) . . . . ?
O1 P1 C13 C18 -140.9(8) . . . . ?
C7 P1 O1 Hf1 61.6(16) . . . . ?
C7 P1 C1 C2 111.2(8) . . . . ?
C7 P1 C1 C6 -67.6(8) . . . . ?
C7 P1 C13 C14 160.1(7) . . . . ?
C7 P1 C13 C18 -20.3(9) . . . . ?
C7 C8 C9 C10 0.4(15) . . . . ?
C7 C12 C11 C10 1.0(15) . . . . ?
C1 P1 O1 Hf1 -58.2(16) . . . . ?
C1 P1 C7 C8 158.9(7) . . . . ?
C1 P1 C7 C12 -24.1(9) . . . . ?
C1 P1 C13 C14 -81.4(8) . . . . ?
C1 P1 C13 C18 98.1(8) . . . . ?
C1 C2 C3 C4 -1.8(17) . . . . ?
C1 C6 C5 C4 1.4(16) . . . . ?
C13 P1 O1 Hf1 -178.5(14) . . . . ?
C13 P1 C7 C8 -81.9(8) . . . . ?
C13 P1 C7 C12 95.0(8) . . . . ?
C13 P1 C1 C2 -7.9(9) . . . . ?
C13 P1 C1 C6 173.4(7) . . . . ?
C13 C14 C15 C16 -0.6(16) . . . . ?
C13 C18 C17 C16 -1.2(16) . . . . ?
C8 C7 C12 C11 1.3(14) . . . . ?
C14 C13 C18 C17 2.1(15) . . . . ?
C14 C15 C16 C17 1.6(17) . . . . ?
C15 C16 C17 C18 -0.7(17) . . . . ?
C12 C7 C8 C9 -1.9(14) . . . . ?
C2 C1 C6 C5 -2.1(15) . . . . ?
C6 C1 C2 C3 2.3(15) . . . . ?
C6 C5 C4 C3 -0.8(17) . . . . ?
C5 C4 C3 C2 1.0(18) . . . . ?
C18 C13 C14 C15 -1.2(14) . . . . ?
C9 C10 C11 C12 -2.6(16) . . . . ?
C11 C10 C9 C8 1.9(16) . . . . ?


_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_original_sample_id CS162_150K
_olex2_submission_special_instructions 'No special instructions were received'
_STOE_detector_distance          '40.0 mm'
_STOE_detector_pixelsize_x       '0.075 mm'
_STOE_detector_pixelsize_y       '0.075 mm'
_STOE_detector_size_x            '8.0 cm'
_STOE_detector_size_y            '7.7 cm'
_STOE_evaluation_integration_A   5.6
_STOE_evaluation_integration_B   -1.0
_STOE_evaluation_integration_EMS 0.019
_STOE_evaluation_LANA_BIS_l_even_max -
_STOE_evaluation_LANA_BIS_l_odd_max -
_STOE_evaluation_LANA_BOS_l_even_max 6
_STOE_evaluation_LANA_BOS_l_odd_max 3
_STOE_evaluation_LANA_completeness 97.4
_STOE_evaluation_LANA_DXS_max_order 1
_STOE_evaluation_LANA_DYS_max_order 1
_STOE_evaluation_LANA_FS_max_order 3
_STOE_evaluation_LANA_max_2theta_available 146.3
_STOE_evaluation_LANA_max_2theta_desired 146.3
_STOE_evaluation_LANA_mean_redundancy 4.3
_STOE_evaluation_LANA_number_refls_after_OR 14943
_STOE_evaluation_LANA_number_refls_outliers 6335
_STOE_evaluation_LANA_number_refls_total 21278
_STOE_evaluation_LANA_number_refls_unique 3445
_STOE_evaluation_LANA_number_refls_written 14943
_STOE_evaluation_LANA_OR_c1      0.035
_STOE_evaluation_LANA_OR_c2      0
_STOE_evaluation_LANA_OR_c3      0
_STOE_evaluation_LANA_OR_c4      0.7
_STOE_evaluation_LANA_point_group -1
_STOE_evaluation_LANA_table      
;
#----------------------------------------------------------------------------
2Theta          16.1   31.5   46.9   62.3   77.7   93.1  108.5  123.9  139.3
#----------------------------------------------------------------------------
<Resolution>    4.69   2.71   1.92   1.46   1.23   1.07   0.95   0.87   0.83
N(total)          64    348    920   2706   4693   4460   3280   3151   1656
<Redundancy>     1.5    2.4    2.8    5.1    6.5    5.3    3.8    3.7    2.8
Complet. [%%]    97.4  100.0  100.0   99.7  100.0  100.0   99.0   98.5   84.6
<I/sigma>      245.2  121.1   97.8   51.6   37.8   32.6   23.4   16.0    8.8
R(int)         0.016  0.019  0.017  0.023  0.025  0.028  0.055  0.125  0.216
#----------------------------------------------------------------------------
;
_STOE_measurement_identifier     CS162_150K
_STOE_measurement_max_exposure_per_frame '6.0 s'
_STOE_measurement_mean_exposure_per_frame '5.8 s'
_STOE_measurement_min_exposure_per_frame '1.0 s'
_STOE_measurement_total_exposure_time '5.9 h'
_STOE_measurement_total_frame_number 3641
_STOE_measurement_total_run_number 34
_STOE_measurement_tube_power     '50.0 W'
####################################################################### 
# 
# 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_cs153_150k
_audit_block_doi                 10.5517/ccdc.csd.cc2dhp4r
_database_code_depnum_ccdc_archive 'CCDC 2219604'
loop_
_citation_id
_citation_doi
_citation_year
1 10.26434/chemrxiv-2023-rcvdn 2023
loop_
_audit_author_name
_audit_author_address
'Alessandro Prescimone'
;University Basel
Switzerland
;
_audit_update_record             
;
2022-11-14 deposited with the CCDC.	2024-05-06 downloaded from the CCDC.
;
_audit_creation_date             2022-09-13
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
carlotta.seno@unibas.ch
alessandro.prescimone@unibas.ch
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C36 H30 Br4 O2 P2 Zr'
_chemical_formula_sum            'C36 H30 Br4 O2 P2 Zr'
_chemical_formula_weight         967.40
_chemical_absolute_configuration ad
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -0.1862 2.2449 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 1 21 1'
_space_group_name_Hall           'P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   9.9980(3)
_cell_length_b                   15.5366(5)
_cell_length_c                   11.8659(3)
_cell_angle_alpha                90
_cell_angle_beta                 100.875(2)
_cell_angle_gamma                90
_cell_volume                     1810.09(9)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    32941
_cell_measurement_temperature    150
_cell_measurement_theta_max      72.62
_cell_measurement_theta_min      4.51
_shelx_estimated_absorpt_T_max   0.541
_shelx_estimated_absorpt_T_min   0.054
_exptl_absorpt_coefficient_mu    8.743
_exptl_absorpt_correction_T_max  0.0270
_exptl_absorpt_correction_T_min  0.0084
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens in: F. R. Ahmed (Editor), "Crystallographic Computing", Munksgaard,
Copenhagen (1970), 255 - 270. Afterwards scaling of reflection intensities was
performed within STOE LANA. J. Koziskova, F. Hahn, J. Richter, J. Kozisek, Acta
Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Finally a spherical absorption correction was done within STOE LANA.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.775
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             944
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
3 10 -5 0.1780
-19 30 15 0.1342
0 -6 1 0.0939
-15 8 0 0.1368
11 30 8 0.0976
-1 -2 -30 0.1809
15 4 6 0.1598
13 -30 -7 0.1401

_exptl_crystal_recrystallization_method 
'The material was recrystallised from DCM by slow evaporation'
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.08
_exptl_crystal_size_rad          0.090
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0446
_diffrn_reflns_av_unetI/netI     0.0361
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            23579
_diffrn_reflns_point_group_measured_fraction_full 0.936
_diffrn_reflns_point_group_measured_fraction_max 0.914
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         72.911
_diffrn_reflns_theta_min         3.793
_diffrn_ambient_temperature      150
_diffrn_detector                 'EIGER2 1M'
_diffrn_detector_area_resol_mean 13.33
_diffrn_detector_type            ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details      
;
 2620 frames, detector distance = 40 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI Cu'
_diffrn_measurement_method       'rotation method, ω scans'
_diffrn_radiation_collimation    '1.2 0.6 mm diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  270
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54186
_diffrn_source                   'Axo Cu'
_diffrn_source_current           1.00
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_reflns_Friedel_coverage         0.777
_reflns_Friedel_fraction_full    0.868
_reflns_Friedel_fraction_max     0.832
_reflns_number_gt                5850
_reflns_number_total             6613
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'X-Area Recipe 1.37.0.0 (STOE, 2021)'
_computing_data_collection       'X-Area Pilatus3_SV 1.31.186.0 (STOE, 2022)'
_computing_data_reduction        
;
X-Area Integrate 2.5.3.0 (STOE, 2021)
X-Area LANA 2.7.5.0 (STOE, 2022)
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.772
_refine_diff_density_min         -1.607
_refine_diff_density_rms         0.279
_refine_ls_abs_structure_details 
;
 Flack x determined using 2197 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.04(4)
_refine_ls_extinction_coef       0.0083(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     407
_refine_ls_number_reflns         6613
_refine_ls_number_restraints     433
_refine_ls_R_factor_all          0.1117
_refine_ls_R_factor_gt           0.0938
_refine_ls_restrained_S_all      1.058
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²+32.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2181
_refine_ls_wR_factor_ref         0.2455
_refine_special_details          
'the aromatic rings needed RIGU and SIMU restraints'
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
C8 \\sim C7 \\sim C12 \\sim C11 \\sim C10 \\sim C9: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
C25 \\sim C30 \\sim C29 \\sim C28 \\sim C27 \\sim C26: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
C14 \\sim C13 \\sim C18 \\sim C17 \\sim C16 \\sim C15: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
C19 \\sim C24 \\sim C23 \\sim C22 \\sim C21 \\sim C20: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
C35 \\sim C36 \\sim C31 \\sim C32 \\sim C33 \\sim C34: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
3. Rigid body (RIGU) restrains
 C13, C18, C17, C16, C15, C14
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C8, C7, C12, C11, C10, C9
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C19, C24, C23, C22, C21, C20
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C26, C27, C28, C29, C30, C25
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C6, C1, C2, C3, C4, C5
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C31, C32, C33, C35, C34, C36
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C32(H32), C36(H36), C6(H6), C26(H26), C35(H35), C30(H30), C20(H20),
 C3(H3), C29(H29), C9(H9), C34(H34), C33(H33), C14(H14), C24(H24), C8(H8),
 C12(H12), C10(H10), C23(H23), C22(H22), C11(H11), C5(H5), C16(H16), C4(H4),
 C18(H18), C21(H21), C28(H28), C17(H17), C27(H27), C15(H15)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zr1 Zr 0.7374(2) 0.44212(15) 0.74426(17) 0.0462(5) Uani 1 1 d . . . . .
Br1 Br 0.8896(3) 0.35997(17) 0.6222(2) 0.0553(7) Uani 1 1 d . . . . .
Br4 Br 0.5658(3) 0.52244(17) 0.8507(2) 0.0541(7) Uani 1 1 d . . . . .
Br2 Br 0.8974(3) 0.57447(16) 0.7668(2) 0.0551(7) Uani 1 1 d . . . . .
Br3 Br 0.5790(3) 0.30469(16) 0.7277(2) 0.0539(7) Uani 1 1 d . . . . .
P2 P 0.5522(6) 0.5525(4) 0.5060(5) 0.0486(13) Uani 1 1 d . . . . .
P1 P 0.9442(6) 0.3856(4) 1.0104(5) 0.0496(13) Uani 1 1 d . . . . .
O1 O 0.8495(15) 0.3940(11) 0.8993(12) 0.047(4) Uani 1 1 d . . . . .
O2 O 0.6247(15) 0.4894(10) 0.5908(11) 0.044(3) Uani 1 1 d . . . . .
C31 C 0.378(2) 0.5606(17) 0.5236(19) 0.049(4) Uani 1 1 d . U . . .
C2 C 1.162(3) 0.3773(19) 0.902(2) 0.056(5) Uani 1 1 d . U . . .
H2 H 1.115904 0.421789 0.854887 0.067 Uiso 1 1 calc R U . . .
C25 C 0.629(2) 0.6525(17) 0.5209(19) 0.051(4) Uani 1 1 d . U . . .
C32 C 0.296(2) 0.6268(17) 0.471(2) 0.051(5) Uani 1 1 d . U . . .
H32 H 0.332853 0.671215 0.431612 0.061 Uiso 1 1 calc R U . . .
C36 C 0.325(3) 0.4959(17) 0.581(2) 0.052(5) Uani 1 1 d . U . . .
H36 H 0.381435 0.450410 0.615855 0.063 Uiso 1 1 calc R U . . .
C6 C 1.170(3) 0.2780(16) 1.057(2) 0.056(5) Uani 1 1 d . U . . .
H6 H 1.128421 0.254220 1.115978 0.067 Uiso 1 1 calc R U . . .
C26 C 0.731(2) 0.6744(18) 0.458(2) 0.055(5) Uani 1 1 d . U . . .
H26 H 0.752017 0.635627 0.401775 0.067 Uiso 1 1 calc R U . . .
C35 C 0.187(3) 0.4974(17) 0.588(2) 0.055(5) Uani 1 1 d . U . . .
H35 H 0.150272 0.453732 0.628854 0.066 Uiso 1 1 calc R U . . .
C19 C 0.550(2) 0.5131(16) 0.365(2) 0.050(5) Uani 1 1 d . U . . .
C30 C 0.606(3) 0.7128(18) 0.608(2) 0.059(5) Uani 1 1 d . U . . .
H30 H 0.538083 0.700944 0.652019 0.071 Uiso 1 1 calc R U . . .
C20 C 0.504(3) 0.5648(18) 0.268(2) 0.058(5) Uani 1 1 d . U . . .
H20 H 0.482029 0.623445 0.278002 0.070 Uiso 1 1 calc R U . . .
C13 C 0.971(3) 0.4850(16) 1.081(2) 0.053(5) Uani 1 1 d . U . . .
C3 C 1.286(2) 0.3480(18) 0.883(2) 0.055(5) Uani 1 1 d . U . . .
H3 H 1.324713 0.371369 0.822659 0.066 Uiso 1 1 calc R U . . .
C1 C 1.105(3) 0.3424(17) 0.987(2) 0.055(5) Uani 1 1 d . U . . .
C29 C 0.682(3) 0.7872(18) 0.628(3) 0.065(6) Uani 1 1 d . U . . .
H29 H 0.666011 0.825369 0.687168 0.078 Uiso 1 1 calc R U . . .
C9 C 0.722(3) 0.1936(19) 1.114(2) 0.063(6) Uani 1 1 d . U . . .
H9 H 0.655933 0.152960 1.078172 0.076 Uiso 1 1 calc R U . . .
C34 C 0.103(2) 0.5622(18) 0.534(2) 0.056(5) Uani 1 1 d . U . . .
H34 H 0.008687 0.562141 0.536013 0.068 Uiso 1 1 calc R U . . .
C33 C 0.159(2) 0.6270(17) 0.479(2) 0.052(5) Uani 1 1 d . U . . .
H33 H 0.102692 0.672737 0.444265 0.062 Uiso 1 1 calc R U . . .
C14 C 0.864(3) 0.5313(19) 1.110(2) 0.061(6) Uani 1 1 d . U . . .
H14 H 0.774973 0.507383 1.091254 0.073 Uiso 1 1 calc R U . . .
C24 C 0.588(3) 0.4270(17) 0.349(2) 0.057(5) Uani 1 1 d . U . . .
H24 H 0.620380 0.390890 0.412537 0.068 Uiso 1 1 calc R U . . .
C8 C 0.774(3) 0.2529(17) 1.048(2) 0.057(5) Uani 1 1 d . U . . .
H8 H 0.744896 0.252661 0.967024 0.068 Uiso 1 1 calc R U . . .
C12 C 0.911(2) 0.313(2) 1.217(2) 0.057(5) Uani 1 1 d . U . . .
H12 H 0.977817 0.352599 1.252411 0.069 Uiso 1 1 calc R U . . .
C10 C 0.765(3) 0.1928(19) 1.232(2) 0.061(6) Uani 1 1 d . U . . .
H10 H 0.732193 0.150353 1.277395 0.073 Uiso 1 1 calc R U . . .
C23 C 0.578(3) 0.397(2) 0.238(2) 0.066(6) Uani 1 1 d . U . . .
H23 H 0.606207 0.339546 0.225987 0.079 Uiso 1 1 calc R U . . .
C7 C 0.869(2) 0.3140(18) 1.100(2) 0.053(5) Uani 1 1 d . U . . .
C22 C 0.526(3) 0.4476(19) 0.146(2) 0.063(6) Uani 1 1 d . U . . .
H22 H 0.514162 0.424600 0.070344 0.076 Uiso 1 1 calc R U . . .
C11 C 0.857(3) 0.2560(19) 1.283(2) 0.062(6) Uani 1 1 d . U . . .
H11 H 0.882902 0.258806 1.363716 0.075 Uiso 1 1 calc R U . . .
C5 C 1.295(3) 0.2488(16) 1.042(2) 0.057(5) Uani 1 1 d . U . . .
H5 H 1.340599 0.204940 1.089901 0.068 Uiso 1 1 calc R U . . .
C16 C 1.013(3) 0.647(2) 1.188(2) 0.072(6) Uani 1 1 d . U . . .
H16 H 1.025369 0.702422 1.221311 0.086 Uiso 1 1 calc R U . . .
C4 C 1.354(3) 0.2842(17) 0.954(2) 0.056(5) Uani 1 1 d . U . . .
H4 H 1.440358 0.264430 0.942211 0.067 Uiso 1 1 calc R U . . .
C18 C 1.108(3) 0.5236(19) 1.112(2) 0.065(6) Uani 1 1 d . U . . .
H18 H 1.185828 0.494580 1.095862 0.079 Uiso 1 1 calc R U . . .
C21 C 0.490(3) 0.534(2) 0.162(2) 0.070(6) Uani 1 1 d . U . . .
H21 H 0.456260 0.568961 0.097236 0.084 Uiso 1 1 calc R U . . .
C28 C 0.781(3) 0.808(2) 0.564(3) 0.077(7) Uani 1 1 d . U . . .
H28 H 0.832942 0.858825 0.579852 0.092 Uiso 1 1 calc R U . . .
C17 C 1.120(3) 0.602(2) 1.165(3) 0.073(7) Uani 1 1 d . U . . .
H17 H 1.208350 0.626779 1.185561 0.087 Uiso 1 1 calc R U . . .
C27 C 0.803(3) 0.754(2) 0.478(3) 0.071(6) Uani 1 1 d . U . . .
H27 H 0.866692 0.769403 0.431482 0.085 Uiso 1 1 calc R U . . .
C15 C 0.880(3) 0.610(2) 1.163(2) 0.070(6) Uani 1 1 d . U . . .
H15 H 0.803845 0.639285 1.181991 0.084 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Zr1 Br1 2.622(3) . ?
Zr1 Br4 2.629(3) . ?
Zr1 Br2 2.588(3) . ?
Zr1 Br3 2.643(3) . ?
Zr1 O1 2.103(13) . ?
Zr1 O2 2.086(13) . ?
P2 O2 1.491(15) . ?
P2 C31 1.80(3) . ?
P2 C25 1.73(3) . ?
P2 C19 1.78(2) . ?
P1 O1 1.477(14) . ?
P1 C13 1.76(3) . ?
P1 C1 1.81(3) . ?
P1 C7 1.80(3) . ?
C31 C32 1.39(3) . ?
C31 C36 1.38(3) . ?
C2 H2 0.9500 . ?
C2 C3 1.37(4) . ?
C2 C1 1.37(3) . ?
C25 C26 1.42(3) . ?
C25 C30 1.44(4) . ?
C32 H32 0.9500 . ?
C32 C33 1.39(3) . ?
C36 H36 0.9500 . ?
C36 C35 1.40(4) . ?
C6 H6 0.9500 . ?
C6 C1 1.38(3) . ?
C6 C5 1.37(4) . ?
C26 H26 0.9500 . ?
C26 C27 1.42(4) . ?
C35 H35 0.9500 . ?
C35 C34 1.38(4) . ?
C19 C20 1.41(3) . ?
C19 C24 1.41(3) . ?
C30 H30 0.9500 . ?
C30 C29 1.38(4) . ?
C20 H20 0.9500 . ?
C20 C21 1.33(3) . ?
C13 C14 1.39(4) . ?
C13 C18 1.47(4) . ?
C3 H3 0.9500 . ?
C3 C4 1.39(3) . ?
C29 H29 0.9500 . ?
C29 C28 1.40(4) . ?
C9 H9 0.9500 . ?
C9 C8 1.37(4) . ?
C9 C10 1.38(4) . ?
C34 H34 0.9500 . ?
C34 C33 1.38(3) . ?
C33 H33 0.9500 . ?
C14 H14 0.9500 . ?
C14 C15 1.37(4) . ?
C24 H24 0.9500 . ?
C24 C23 1.38(3) . ?
C8 H8 0.9500 . ?
C8 C7 1.40(4) . ?
C12 H12 0.9500 . ?
C12 C7 1.37(3) . ?
C12 C11 1.35(4) . ?
C10 H10 0.9500 . ?
C10 C11 1.41(4) . ?
C23 H23 0.9500 . ?
C23 C22 1.37(4) . ?
C22 H22 0.9500 . ?
C22 C21 1.40(4) . ?
C11 H11 0.9500 . ?
C5 H5 0.9500 . ?
C5 C4 1.41(4) . ?
C16 H16 0.9500 . ?
C16 C17 1.35(4) . ?
C16 C15 1.42(4) . ?
C4 H4 0.9500 . ?
C18 H18 0.9500 . ?
C18 C17 1.37(4) . ?
C21 H21 0.9500 . ?
C28 H28 0.9500 . ?
C28 C27 1.37(5) . ?
C17 H17 0.9500 . ?
C27 H27 0.9500 . ?
C15 H15 0.9500 . ?

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
Br1 Zr1 Br4 174.70(11) . . ?
Br1 Zr1 Br3 88.15(10) . . ?
Br4 Zr1 Br3 89.03(10) . . ?
Br2 Zr1 Br1 91.82(11) . . ?
Br2 Zr1 Br4 91.15(11) . . ?
Br2 Zr1 Br3 178.04(12) . . ?
O1 Zr1 Br1 92.3(5) . . ?
O1 Zr1 Br4 92.1(5) . . ?
O1 Zr1 Br2 88.6(5) . . ?
O1 Zr1 Br3 89.5(5) . . ?
O2 Zr1 Br1 87.9(4) . . ?
O2 Zr1 Br4 87.6(4) . . ?
O2 Zr1 Br2 91.8(4) . . ?
O2 Zr1 Br3 90.1(4) . . ?
O2 Zr1 O1 179.5(7) . . ?
O2 P2 C31 109.0(10) . . ?
O2 P2 C25 111.9(10) . . ?
O2 P2 C19 109.1(10) . . ?
C25 P2 C31 110.1(12) . . ?
C25 P2 C19 109.5(11) . . ?
C19 P2 C31 107.1(11) . . ?
O1 P1 C13 111.5(11) . . ?
O1 P1 C1 109.6(11) . . ?
O1 P1 C7 108.3(10) . . ?
C13 P1 C1 109.7(12) . . ?
C13 P1 C7 107.7(11) . . ?
C7 P1 C1 110.0(11) . . ?
P1 O1 Zr1 163.4(11) . . ?
P2 O2 Zr1 159.1(10) . . ?
C32 C31 P2 120.4(19) . . ?
C36 C31 P2 118.7(19) . . ?
C36 C31 C32 121(2) . . ?
C3 C2 H2 120.0 . . ?
C1 C2 H2 120.0 . . ?
C1 C2 C3 120(2) . . ?
C26 C25 P2 121(2) . . ?
C26 C25 C30 117(2) . . ?
C30 C25 P2 122.2(19) . . ?
C31 C32 H32 120.6 . . ?
C33 C32 C31 119(2) . . ?
C33 C32 H32 120.6 . . ?
C31 C36 H36 120.2 . . ?
C31 C36 C35 120(2) . . ?
C35 C36 H36 120.2 . . ?
C1 C6 H6 120.3 . . ?
C5 C6 H6 120.3 . . ?
C5 C6 C1 119(2) . . ?
C25 C26 H26 119.7 . . ?
C25 C26 C27 121(3) . . ?
C27 C26 H26 119.7 . . ?
C36 C35 H35 119.8 . . ?
C34 C35 C36 120(2) . . ?
C34 C35 H35 119.8 . . ?
C20 C19 P2 121.2(19) . . ?
C20 C19 C24 119(2) . . ?
C24 C19 P2 120.0(18) . . ?
C25 C30 H30 119.5 . . ?
C29 C30 C25 121(3) . . ?
C29 C30 H30 119.5 . . ?
C19 C20 H20 119.2 . . ?
C21 C20 C19 122(3) . . ?
C21 C20 H20 119.2 . . ?
C14 C13 P1 121(2) . . ?
C14 C13 C18 117(2) . . ?
C18 C13 P1 122(2) . . ?
C2 C3 H3 120.2 . . ?
C2 C3 C4 120(2) . . ?
C4 C3 H3 120.2 . . ?
C2 C1 P1 118(2) . . ?
C2 C1 C6 122(3) . . ?
C6 C1 P1 120.4(19) . . ?
C30 C29 H29 119.5 . . ?
C30 C29 C28 121(3) . . ?
C28 C29 H29 119.5 . . ?
C8 C9 H9 120.0 . . ?
C8 C9 C10 120(3) . . ?
C10 C9 H9 120.0 . . ?
C35 C34 H34 120.5 . . ?
C33 C34 C35 119(2) . . ?
C33 C34 H34 120.5 . . ?
C32 C33 H33 119.3 . . ?
C34 C33 C32 121(2) . . ?
C34 C33 H33 119.3 . . ?
C13 C14 H14 118.5 . . ?
C15 C14 C13 123(3) . . ?
C15 C14 H14 118.5 . . ?
C19 C24 H24 120.6 . . ?
C23 C24 C19 119(2) . . ?
C23 C24 H24 120.6 . . ?
C9 C8 H8 119.8 . . ?
C9 C8 C7 120(2) . . ?
C7 C8 H8 119.8 . . ?
C7 C12 H12 119.5 . . ?
C11 C12 H12 119.5 . . ?
C11 C12 C7 121(3) . . ?
C9 C10 H10 120.6 . . ?
C9 C10 C11 119(2) . . ?
C11 C10 H10 120.6 . . ?
C24 C23 H23 119.7 . . ?
C22 C23 C24 121(3) . . ?
C22 C23 H23 119.7 . . ?
C8 C7 P1 119.0(18) . . ?
C12 C7 P1 122(2) . . ?
C12 C7 C8 119(2) . . ?
C23 C22 H22 119.7 . . ?
C23 C22 C21 121(2) . . ?
C21 C22 H22 119.7 . . ?
C12 C11 C10 121(3) . . ?
C12 C11 H11 119.7 . . ?
C10 C11 H11 119.7 . . ?
C6 C5 H5 120.3 . . ?
C6 C5 C4 119(2) . . ?
C4 C5 H5 120.3 . . ?
C17 C16 H16 120.1 . . ?
C17 C16 C15 120(3) . . ?
C15 C16 H16 120.1 . . ?
C3 C4 C5 120(2) . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
C13 C18 H18 120.8 . . ?
C17 C18 C13 118(3) . . ?
C17 C18 H18 120.8 . . ?
C20 C21 C22 119(3) . . ?
C20 C21 H21 120.3 . . ?
C22 C21 H21 120.3 . . ?
C29 C28 H28 120.0 . . ?
C27 C28 C29 120(3) . . ?
C27 C28 H28 120.0 . . ?
C16 C17 C18 123(3) . . ?
C16 C17 H17 118.5 . . ?
C18 C17 H17 118.5 . . ?
C26 C27 H27 119.8 . . ?
C28 C27 C26 120(3) . . ?
C28 C27 H27 119.8 . . ?
C14 C15 C16 119(3) . . ?
C14 C15 H15 120.7 . . ?
C16 C15 H15 120.7 . . ?

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
P2 C31 C32 C33 174(2) . . . . ?
P2 C31 C36 C35 -174.9(19) . . . . ?
P2 C25 C26 C27 -174(2) . . . . ?
P2 C25 C30 C29 171(2) . . . . ?
P2 C19 C20 C21 -174(2) . . . . ?
P2 C19 C24 C23 176(2) . . . . ?
P1 C13 C14 C15 -178(2) . . . . ?
P1 C13 C18 C17 178(2) . . . . ?
O1 P1 C13 C14 59(2) . . . . ?
O1 P1 C13 C18 -120(2) . . . . ?
O1 P1 C1 C2 47(2) . . . . ?
O1 P1 C1 C6 -136(2) . . . . ?
O1 P1 C7 C8 25(2) . . . . ?
O1 P1 C7 C12 -160(2) . . . . ?
O2 P2 C31 C32 167.2(19) . . . . ?
O2 P2 C31 C36 -19(2) . . . . ?
O2 P2 C25 C26 91.1(19) . . . . ?
O2 P2 C25 C30 -80(2) . . . . ?
O2 P2 C19 C20 -172(2) . . . . ?
O2 P2 C19 C24 12(2) . . . . ?
C31 P2 O2 Zr1 -89(3) . . . . ?
C31 P2 C25 C26 -147.5(18) . . . . ?
C31 P2 C25 C30 41(2) . . . . ?
C31 P2 C19 C20 71(2) . . . . ?
C31 P2 C19 C24 -106(2) . . . . ?
C31 C32 C33 C34 -1(4) . . . . ?
C31 C36 C35 C34 2(4) . . . . ?
C2 C3 C4 C5 1(4) . . . . ?
C25 P2 O2 Zr1 33(3) . . . . ?
C25 P2 C31 C32 44(2) . . . . ?
C25 P2 C31 C36 -141.7(19) . . . . ?
C25 P2 C19 C20 -49(2) . . . . ?
C25 P2 C19 C24 135(2) . . . . ?
C25 C26 C27 C28 5(4) . . . . ?
C25 C30 C29 C28 1(4) . . . . ?
C32 C31 C36 C35 -1(4) . . . . ?
C36 C31 C32 C33 0(4) . . . . ?
C36 C35 C34 C33 -3(4) . . . . ?
C6 C5 C4 C3 0(4) . . . . ?
C26 C25 C30 C29 0(4) . . . . ?
C35 C34 C33 C32 2(4) . . . . ?
C19 P2 O2 Zr1 154(3) . . . . ?
C19 P2 C31 C32 -75(2) . . . . ?
C19 P2 C31 C36 99(2) . . . . ?
C19 P2 C25 C26 -30(2) . . . . ?
C19 P2 C25 C30 159(2) . . . . ?
C19 C20 C21 C22 -2(5) . . . . ?
C19 C24 C23 C22 -3(4) . . . . ?
C30 C25 C26 C27 -2(3) . . . . ?
C30 C29 C28 C27 1(5) . . . . ?
C20 C19 C24 C23 -1(4) . . . . ?
C13 P1 O1 Zr1 27(4) . . . . ?
C13 P1 C1 C2 -76(2) . . . . ?
C13 P1 C1 C6 102(2) . . . . ?
C13 P1 C7 C8 146(2) . . . . ?
C13 P1 C7 C12 -40(3) . . . . ?
C13 C14 C15 C16 1(4) . . . . ?
C13 C18 C17 C16 -1(5) . . . . ?
C3 C2 C1 P1 178(2) . . . . ?
C3 C2 C1 C6 0(4) . . . . ?
C1 P1 O1 Zr1 -94(4) . . . . ?
C1 P1 C13 C14 -180(2) . . . . ?
C1 P1 C13 C18 1(2) . . . . ?
C1 P1 C7 C8 -95(2) . . . . ?
C1 P1 C7 C12 80(2) . . . . ?
C1 C2 C3 C4 -1(4) . . . . ?
C1 C6 C5 C4 -1(4) . . . . ?
C29 C28 C27 C26 -4(5) . . . . ?
C9 C8 C7 P1 176(2) . . . . ?
C9 C8 C7 C12 1(4) . . . . ?
C9 C10 C11 C12 -4(4) . . . . ?
C14 C13 C18 C17 -1(4) . . . . ?
C24 C19 C20 C21 3(4) . . . . ?
C24 C23 C22 C21 4(5) . . . . ?
C8 C9 C10 C11 3(4) . . . . ?
C10 C9 C8 C7 -1(4) . . . . ?
C23 C22 C21 C20 -1(5) . . . . ?
C7 P1 O1 Zr1 146(4) . . . . ?
C7 P1 C13 C14 -60(2) . . . . ?
C7 P1 C13 C18 121(2) . . . . ?
C7 P1 C1 C2 166(2) . . . . ?
C7 P1 C1 C6 -17(3) . . . . ?
C7 C12 C11 C10 4(4) . . . . ?
C11 C12 C7 P1 -177(2) . . . . ?
C11 C12 C7 C8 -2(4) . . . . ?
C5 C6 C1 P1 -177(2) . . . . ?
C5 C6 C1 C2 1(4) . . . . ?
C18 C13 C14 C15 1(4) . . . . ?
C17 C16 C15 C14 -3(4) . . . . ?
C15 C16 C17 C18 3(5) . . . . ?


_olex2_date_sample_data_collection 2022-09-10
_olex2_date_sample_submission    2022-09-05
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a mylar loop in perfluoroether oil'
_olex2_submission_original_sample_id CS153_150K
_olex2_submission_special_instructions 'No special instructions were received'
_STOE_detector_distance          '40.0 mm'
_STOE_detector_pixelsize_x       '0.075 mm'
_STOE_detector_pixelsize_y       '0.075 mm'
_STOE_detector_size_x            '8.0 cm'
_STOE_detector_size_y            '7.7 cm'
_STOE_evaluation_integration_A   5.6
_STOE_evaluation_integration_B   -1.0
_STOE_evaluation_integration_EMS 0.017
_STOE_evaluation_LANA_BIS_l_even_max -
_STOE_evaluation_LANA_BIS_l_odd_max -
_STOE_evaluation_LANA_BOS_l_even_max 6
_STOE_evaluation_LANA_BOS_l_odd_max 3
_STOE_evaluation_LANA_completeness 91.4
_STOE_evaluation_LANA_DXS_max_order 1
_STOE_evaluation_LANA_DYS_max_order 1
_STOE_evaluation_LANA_FS_max_order 3
_STOE_evaluation_LANA_max_2theta_available 145.9
_STOE_evaluation_LANA_max_2theta_desired 145.9
_STOE_evaluation_LANA_mean_redundancy 3.6
_STOE_evaluation_LANA_number_refls_after_OR 23593
_STOE_evaluation_LANA_number_refls_outliers 8510
_STOE_evaluation_LANA_number_refls_total 32103
_STOE_evaluation_LANA_number_refls_unique 6621
_STOE_evaluation_LANA_number_refls_written 23593
_STOE_evaluation_LANA_OR_c1      0.035
_STOE_evaluation_LANA_OR_c2      0
_STOE_evaluation_LANA_OR_c3      0
_STOE_evaluation_LANA_OR_c4      0.7
_STOE_evaluation_LANA_point_group 2
_STOE_evaluation_LANA_table      
;
#--------------------------------------
2Theta          14.3   29.9   45.5   61.1   76.7   92.3  107.9  123.5  139.1
#--------------------------------------
<Resolution>    5.26   2.88   1.97   1.47   1.24   1.07   0.95   0.88   0.83
N(total)          70    452   1102   3740   6646   6903   4905   5414   2871
<Redundancy>     1.2    1.8    1.9    3.7    4.8    4.5    3.2    3.5    2.8
Complet. [%%]    91.2   96.8  100.0   98.3   98.6   95.2   89.8   88.6   75.0
<I/sigma>      136.8   84.9   55.1   28.4   23.4   17.9   12.5    9.4    5.5
R(int)         0.017  0.028  0.030  0.039  0.036  0.042  0.081  0.167  0.287
#--------------------------------------
;
_STOE_measurement_identifier     CS153_150K
_STOE_measurement_max_exposure_per_frame '8.0 s'
_STOE_measurement_mean_exposure_per_frame '7.7 s'
_STOE_measurement_min_exposure_per_frame '2.0 s'
_STOE_measurement_total_exposure_time '5.6 h'
_STOE_measurement_total_frame_number 2620
_STOE_measurement_total_run_number 23
_STOE_measurement_tube_power     '50.0 W'
_vrf_PLAT342_cs153_150k          
;
PROBLEM: Low Bond Precision on C-C Bonds ............... 0.03833 Ang. 
RESPONSE: this is probably due to the presence of many heavy atoms in
combination with a copper source diffractometer. A small crystal has been
used and indexed,the extinction parameter has been refined. This was,
however not enough to avoid these problems.
;
_vrf_PLAT939_cs153_150k          
;
PROBLEM: Large Value of Not (SHELXL) Weight Optimized S . 178.90 Check
RESPONSE: this is probably due to the presence of many heavy atoms in
combination with a copper source diffractometer. A small crystal has been
used and indexed,the extinction parameter has been refined. This was,
however not enough to avoid these problems.
;
