# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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_scc140_0m
_database_code_depnum_ccdc_archive 'CCDC 2015378'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/D0SC03777J 2020
loop_
_audit_author_name
_audit_author_address
'Scott Coste'
;Northwestern University
United States of America
;
_audit_update_record             
;
2020-07-09 deposited with the CCDC.	2020-09-08 downloaded from the CCDC.
;
_audit_creation_date             2019-03-08
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        
'hydrotris(3-phenyl-5-methylpyrazolyl)borate nickel triphenylstannide'
_chemical_formula_moiety         'C48 H43 B1 N6 Ni1 Sn1'
_chemical_formula_sum            'C54 H49 B N6 Ni Sn'
_chemical_formula_weight         970.20
_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 0.0033 0.0016 '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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sn Sn -0.6537 1.4246 '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      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3'
_space_group_name_Hall           '-R 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   12.3186(4)
_cell_length_b                   12.3186(4)
_cell_length_c                   49.0829(17)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     6450.4(5)
_cell_formula_units_Z            6
_cell_measurement_reflns_used    9884
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      30.334
_cell_measurement_theta_min      2.490
_shelx_estimated_absorpt_T_max   0.955
_shelx_estimated_absorpt_T_min   0.650
_exptl_absorpt_coefficient_mu    1.066
_exptl_absorpt_correction_T_max  0.8872
_exptl_absorpt_correction_T_min  0.6505
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1608 before and 0.0827 after correction. The Ratio of minimum to maximum transmission is 0.7332. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear bluish green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   bluish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.499
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             2988
_exptl_crystal_preparation       
'Synthesized by the reaction of HSnPh3 with [TpNiCH2SiMe3].,Magnetic properties'
_exptl_crystal_recrystallization_method 
'Crystallized from a benzene/hexanes layering.'
_exptl_crystal_size_max          0.443
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.044
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0891
_diffrn_reflns_av_unetI/netI     0.0329
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       69
_diffrn_reflns_limit_l_min       -70
_diffrn_reflns_number            65036
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.605
_diffrn_reflns_theta_min         1.245
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_special_details          ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3715
_reflns_number_total             4430
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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       'SAINT V8.38A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_refine_diff_density_max         0.605
_refine_diff_density_min         -0.900
_refine_diff_density_rms         0.072
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         4430
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0327
_refine_ls_restrained_S_all      1.050
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0371P)²+11.5138P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0823
_refine_ls_wR_factor_ref         0.0871
_refine_special_details          
'Refined with a solvent mask due to benzene molecule disordered over a special position.,SQUEEZE'
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 B1(H1)
2.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C6(H6), C8(H8), C13(H13), C12(H12), C3(H3), C14(H14), C10(H10),
 C9(H9), C16(H16), C15(H15)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C)
;
_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
Sn1 Sn 0.333333 0.666667 0.39520(2) 0.02855(7) Uani 1 3 d S T P . .
Ni1 Ni 0.333333 0.666667 0.44958(2) 0.02258(9) Uani 1 3 d S T P . .
N2 N 0.32681(14) 0.54654(14) 0.50020(3) 0.0228(3) Uani 1 1 d . . . . .
N1 N 0.30083(15) 0.51758(14) 0.47301(3) 0.0231(3) Uani 1 1 d . . . . .
C7 C 0.14839(19) 0.2732(2) 0.40097(4) 0.0324(4) Uani 1 1 d . . . . .
H7 H 0.091939 0.277362 0.388400 0.039 Uiso 1 1 calc R . . . .
C5 C 0.2627(2) 0.3383(2) 0.44325(4) 0.0326(4) Uani 1 1 d . . . . .
C6 C 0.18072(18) 0.34427(19) 0.42469(4) 0.0284(4) Uani 1 1 d . . . . .
H6 H 0.146630 0.397077 0.428214 0.034 Uiso 1 1 calc R . . . .
C8 C 0.1978(2) 0.1966(2) 0.39556(4) 0.0394(5) Uani 1 1 d . . . . .
H8 H 0.174697 0.147700 0.379393 0.047 Uiso 1 1 calc R . . . .
C2 C 0.3403(2) 0.4574(2) 0.51291(4) 0.0343(4) Uani 1 1 d . . . . .
C13 C 0.4953(3) 1.0728(2) 0.37888(5) 0.0429(5) Uani 1 1 d . . . . .
H13 H 0.552901 1.147499 0.388101 0.051 Uiso 1 1 calc R . . . .
C4 C 0.2948(2) 0.4066(2) 0.46942(4) 0.0321(4) Uani 1 1 d . . . . .
C11 C 0.3852(2) 0.8455(2) 0.37609(4) 0.0328(4) Uani 1 1 d . . . . .
C1 C 0.3726(3) 0.4623(2) 0.54235(4) 0.0422(6) Uani 1 1 d . . . . .
H1A H 0.463513 0.499341 0.544304 0.063 Uiso 1 1 calc GR . . . .
H1B H 0.330339 0.377230 0.549875 0.063 Uiso 1 1 calc GR . . . .
H1C H 0.345217 0.513606 0.552210 0.063 Uiso 1 1 calc GR . . . .
C12 C 0.4698(2) 0.9572(2) 0.38886(4) 0.0348(4) Uani 1 1 d . . . . .
H12 H 0.511377 0.954027 0.404893 0.042 Uiso 1 1 calc R . . . .
C3 C 0.3196(3) 0.3662(2) 0.49403(4) 0.0494(7) Uani 1 1 d . . . . .
H3 H 0.321820 0.291209 0.497125 0.059 Uiso 1 1 calc R . . . .
C14 C 0.4358(3) 1.0790(3) 0.35523(5) 0.0485(6) Uani 1 1 d . . . . .
H14 H 0.451140 1.157694 0.348471 0.058 Uiso 1 1 calc R . . . .
C10 C 0.3124(3) 0.2610(2) 0.43754(5) 0.0474(6) Uani 1 1 d . . . . .
H10 H 0.368454 0.255953 0.450096 0.057 Uiso 1 1 calc R . . . .
C9 C 0.2807(3) 0.1912(2) 0.41366(5) 0.0483(6) Uani 1 1 d . . . . .
H9 H 0.315977 0.139715 0.409786 0.058 Uiso 1 1 calc R . . . .
C16 C 0.3294(2) 0.8543(2) 0.35195(4) 0.0419(5) Uani 1 1 d . . . . .
H16 H 0.273262 0.780091 0.342366 0.050 Uiso 1 1 calc R . . . .
C15 C 0.3550(3) 0.9704(3) 0.34181(4) 0.0487(6) Uani 1 1 d . . . . .
H15 H 0.316110 0.974373 0.325423 0.058 Uiso 1 1 calc R . . . .
B1 B 0.333333 0.666667 0.51124(6) 0.0217(6) Uani 1 3 d S T P . .
H1 H 0.333333 0.666660 0.531616 0.026 Uiso 1 3 calc RS T P . .


_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
Sn1 Ni1 2.6693(4) . ?
Sn1 C11 2.176(2) 3_565 ?
Sn1 C11 2.176(2) 2_665 ?
Sn1 C11 2.176(2) . ?
Ni1 N1 2.0298(15) . ?
Ni1 N1 2.0297(15) 3_565 ?
Ni1 N1 2.0297(15) 2_665 ?
N2 N1 1.3776(19) . ?
N2 C2 1.343(2) . ?
N2 B1 1.5397(18) . ?
N1 C4 1.343(2) . ?
C7 H7 0.9500 . ?
C7 C6 1.390(3) . ?
C7 C8 1.380(3) . ?
C5 C6 1.389(3) . ?
C5 C4 1.477(3) . ?
C5 C10 1.395(3) . ?
C6 H6 0.9500 . ?
C8 H8 0.9500 . ?
C8 C9 1.380(3) . ?
C2 C1 1.492(3) . ?
C2 C3 1.378(3) . ?
C13 H13 0.9500 . ?
C13 C12 1.386(3) . ?
C13 C14 1.395(4) . ?
C4 C3 1.398(3) . ?
C11 C12 1.392(3) . ?
C11 C16 1.401(3) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C12 H12 0.9500 . ?
C3 H3 0.9500 . ?
C14 H14 0.9500 . ?
C14 C15 1.372(4) . ?
C10 H10 0.9500 . ?
C10 C9 1.389(3) . ?
C9 H9 0.9500 . ?
C16 H16 0.9500 . ?
C16 C15 1.393(4) . ?
C15 H15 0.9500 . ?
B1 H1 1.0000 . ?

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
C11 Sn1 Ni1 115.54(5) 2_665 . ?
C11 Sn1 Ni1 115.54(5) . . ?
C11 Sn1 Ni1 115.54(5) 3_565 . ?
C11 Sn1 C11 102.78(6) 2_665 3_565 ?
C11 Sn1 C11 102.78(6) . 3_565 ?
C11 Sn1 C11 102.78(6) 2_665 . ?
N1 Ni1 Sn1 124.50(4) 3_565 . ?
N1 Ni1 Sn1 124.50(4) . . ?
N1 Ni1 Sn1 124.50(4) 2_665 . ?
N1 Ni1 N1 91.07(6) 2_665 . ?
N1 Ni1 N1 91.07(6) 3_565 . ?
N1 Ni1 N1 91.07(6) 3_565 2_665 ?
N1 N2 B1 118.93(16) . . ?
C2 N2 N1 110.23(15) . . ?
C2 N2 B1 130.83(16) . . ?
N2 N1 Ni1 113.54(11) . . ?
C4 N1 Ni1 137.06(13) . . ?
C4 N1 N2 106.15(14) . . ?
C6 C7 H7 119.8 . . ?
C8 C7 H7 119.8 . . ?
C8 C7 C6 120.43(19) . . ?
C6 C5 C4 122.38(18) . . ?
C6 C5 C10 118.92(18) . . ?
C10 C5 C4 118.64(18) . . ?
C7 C6 H6 119.9 . . ?
C5 C6 C7 120.21(19) . . ?
C5 C6 H6 119.9 . . ?
C7 C8 H8 120.0 . . ?
C7 C8 C9 119.96(19) . . ?
C9 C8 H8 120.0 . . ?
N2 C2 C1 123.79(18) . . ?
N2 C2 C3 107.84(17) . . ?
C3 C2 C1 128.38(19) . . ?
C12 C13 H13 120.2 . . ?
C12 C13 C14 119.7(2) . . ?
C14 C13 H13 120.2 . . ?
N1 C4 C5 123.80(17) . . ?
N1 C4 C3 109.78(17) . . ?
C3 C4 C5 126.39(19) . . ?
C12 C11 Sn1 120.13(14) . . ?
C12 C11 C16 117.3(2) . . ?
C16 C11 Sn1 122.41(17) . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C13 C12 C11 121.9(2) . . ?
C13 C12 H12 119.0 . . ?
C11 C12 H12 119.0 . . ?
C2 C3 C4 105.97(18) . . ?
C2 C3 H3 127.0 . . ?
C4 C3 H3 127.0 . . ?
C13 C14 H14 120.3 . . ?
C15 C14 C13 119.4(2) . . ?
C15 C14 H14 120.3 . . ?
C5 C10 H10 119.7 . . ?
C9 C10 C5 120.5(2) . . ?
C9 C10 H10 119.7 . . ?
C8 C9 C10 119.9(2) . . ?
C8 C9 H9 120.0 . . ?
C10 C9 H9 120.0 . . ?
C11 C16 H16 119.6 . . ?
C15 C16 C11 120.9(2) . . ?
C15 C16 H16 119.6 . . ?
C14 C15 C16 120.7(2) . . ?
C14 C15 H15 119.6 . . ?
C16 C15 H15 119.6 . . ?
N2 B1 N2 108.32(12) 3_565 . ?
N2 B1 N2 108.33(12) 3_565 2_665 ?
N2 B1 N2 108.32(12) 2_665 . ?
N2 B1 H1 110.6 3_565 . ?
N2 B1 H1 110.6 2_665 . ?
N2 B1 H1 110.6 . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 0.000 71.4 0.0 ?
2 0.000 0.000 0.354 10.8 0.0 ?
3 0.000 0.000 0.500 169.6 42.2 '1 benzene'
4 0.000 0.000 0.646 10.8 0.0 ?
5 0.333 0.667 0.167 169.6 42.2 '1 benzene'
6 0.333 0.667 0.667 71.4 0.0 ?
7 0.333 0.667 0.021 10.8 0.0 ?
8 0.333 0.667 0.312 10.8 0.0 ?
9 0.667 0.333 0.833 169.6 41.7 '1 benzene'
10 0.667 0.333 0.333 71.4 0.0 ?
11 0.667 0.333 0.688 10.8 0.0 ?
12 0.667 0.333 0.979 10.8 0.0 ?

_olex2_exptl_crystal_mounting_method 
'Mounted on a MicroMount rod with Paratone-N oil.'
_olex2_submission_special_instructions 'No special instructions were received'
_chemical_properties_physical    Moisture-sensitive
####################################################################### 
# 
# 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_mo_scc143_0m
_database_code_depnum_ccdc_archive 'CCDC 2015381'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/D0SC03777J 2020
loop_
_audit_author_name
_audit_author_address
'Scott Coste'
;Northwestern University
United States of America
;
_audit_update_record             
;
2020-07-09 deposited with the CCDC.	2020-09-08 downloaded from the CCDC.
;
_audit_creation_date             2018-11-27
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        
'hydrotris(3-phenyl-5-methylpyrazolyl)borate zinc(II) chloride'
_chemical_formula_moiety         'C30 H28 B Cl N6 Zn'
_chemical_formula_sum            'C30 H28 B Cl N6 Zn'
_chemical_formula_weight         584.21
_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 0.0033 0.0016 '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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 '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           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   11.0364(8)
_cell_length_b                   15.2242(13)
_cell_length_c                   16.1001(13)
_cell_angle_alpha                90
_cell_angle_beta                 94.548(2)
_cell_angle_gamma                90
_cell_volume                     2696.6(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4835
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.382
_cell_measurement_theta_min      2.326
_shelx_estimated_absorpt_T_max   0.960
_shelx_estimated_absorpt_T_min   0.713
_exptl_absorpt_coefficient_mu    1.042
_exptl_absorpt_correction_T_max  0.4932
_exptl_absorpt_correction_T_min  0.4028
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0620 before and 0.0530 after correction. The Ratio of minimum to maximum transmission is 0.8167. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.439
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1208
_exptl_crystal_preparation       'Synthesized by reacting KTp with ZnCl2.'
_exptl_crystal_recrystallization_method 
'Crystallized from dichloromethane/hexane layering.'
_exptl_crystal_size_max          0.348
_exptl_crystal_size_mid          0.122
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0855
_diffrn_reflns_av_unetI/netI     0.0719
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            44426
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.210
_diffrn_reflns_theta_min         1.844
_diffrn_ambient_temperature      100.11
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  Triumph
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5269
_reflns_number_total             7978
_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       'SAINT V8.34A (Bruker, 2017)'
_computing_data_collection       'APEX2 V2017.3 (Bruker, 2017)'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_refine_diff_density_max         0.720
_refine_diff_density_min         -0.685
_refine_diff_density_rms         0.093
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     355
_refine_ls_number_reflns         7978
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0926
_refine_ls_R_factor_gt           0.0469
_refine_ls_restrained_S_all      1.010
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0432P)²+1.4335P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0900
_refine_ls_wR_factor_ref         0.1048
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 B1(H1)
2.b Aromatic/amide H refined with riding coordinates:
 C23(H23), C13(H13), C10(H10), C6(H6), C3(H3), C20(H20), C7(H7), C16(H16),
 C30(H30), C26(H26), C9(H9), C8(H8), C28(H28), C29(H29), C17(H17), C19(H19),
 C27(H27), C18(H18)
2.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C11(H11A,H11B,H11C), C1(H1A,H1B,H1C)
;
_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
Zn1 Zn 0.21719(2) 0.75382(2) 0.73114(2) 0.01218(7) Uani 1 1 d . . . . .
Cl1 Cl 0.03279(5) 0.79323(4) 0.68994(4) 0.01730(13) Uani 1 1 d . . . . .
N3 N 0.28804(16) 0.75539(14) 0.85199(12) 0.0127(4) Uani 1 1 d . . . . .
N6 N 0.39293(16) 0.61710(14) 0.74304(12) 0.0130(4) Uani 1 1 d . . . . .
N5 N 0.26968(16) 0.62599(14) 0.72355(12) 0.0137(4) Uani 1 1 d . . . . .
N4 N 0.40769(17) 0.73073(13) 0.85781(12) 0.0127(4) Uani 1 1 d . . . . .
N2 N 0.47177(17) 0.76748(13) 0.71461(12) 0.0136(4) Uani 1 1 d . . . . .
N1 N 0.36591(16) 0.80594(13) 0.68111(12) 0.0132(4) Uani 1 1 d . . . . .
C22 C 0.4289(2) 0.53634(16) 0.72084(14) 0.0134(5) Uani 1 1 d . . . . .
C23 C 0.3283(2) 0.49130(17) 0.68650(14) 0.0145(5) Uani 1 1 d . . . . .
H23 H 0.326079 0.433335 0.664589 0.017 Uiso 1 1 calc R . . . .
C15 C 0.1379(2) 0.80361(16) 0.94795(14) 0.0146(5) Uani 1 1 d . . . . .
C12 C 0.4558(2) 0.73961(16) 0.93731(14) 0.0141(5) Uani 1 1 d . . . . .
C14 C 0.2614(2) 0.77789(16) 0.92916(15) 0.0128(5) Uani 1 1 d . . . . .
C13 C 0.3651(2) 0.76938(15) 0.98416(15) 0.0148(5) Uani 1 1 d . . . . .
H13 H 0.371703 0.781650 1.042196 0.018 Uiso 1 1 calc R . . . .
C10 C 0.2162(2) 0.95697(17) 0.60311(15) 0.0163(5) Uani 1 1 d . . . . .
H10 H 0.199177 0.944174 0.658747 0.020 Uiso 1 1 calc R . . . .
C25 C 0.1008(2) 0.52947(16) 0.67273(15) 0.0144(5) Uani 1 1 d . . . . .
C6 C 0.3362(2) 0.93465(17) 0.48671(15) 0.0169(5) Uani 1 1 d . . . . .
H6 H 0.402409 0.907275 0.462675 0.020 Uiso 1 1 calc R . . . .
C3 C 0.5221(2) 0.85144(17) 0.61157(15) 0.0163(5) Uani 1 1 d . . . . .
H3 H 0.567397 0.880537 0.571990 0.020 Uiso 1 1 calc R . . . .
C2 C 0.5664(2) 0.79505(17) 0.67285(15) 0.0154(5) Uani 1 1 d . . . . .
C24 C 0.2307(2) 0.54913(16) 0.69084(14) 0.0133(5) Uani 1 1 d . . . . .
C5 C 0.3135(2) 0.91585(16) 0.56880(14) 0.0141(5) Uani 1 1 d . . . . .
C4 C 0.3972(2) 0.85773(16) 0.61874(14) 0.0139(5) Uani 1 1 d . . . . .
C21 C 0.5575(2) 0.50549(17) 0.73457(16) 0.0181(5) Uani 1 1 d . . . . .
H21A H 0.610939 0.546321 0.707815 0.027 Uiso 1 1 calc GR . . . .
H21B H 0.564639 0.446817 0.710397 0.027 Uiso 1 1 calc GR . . . .
H21C H 0.581161 0.503093 0.794487 0.027 Uiso 1 1 calc GR . . . .
C11 C 0.5840(2) 0.71736(18) 0.96428(16) 0.0180(5) Uani 1 1 d . . . . .
H11A H 0.596724 0.654146 0.957516 0.027 Uiso 1 1 calc GR . . . .
H11B H 0.601283 0.733422 1.022964 0.027 Uiso 1 1 calc GR . . . .
H11C H 0.638441 0.749847 0.930146 0.027 Uiso 1 1 calc GR . . . .
C20 C 0.0361(2) 0.76454(17) 0.90695(15) 0.0175(5) Uani 1 1 d . . . . .
H20 H 0.045762 0.721149 0.865575 0.021 Uiso 1 1 calc R . . . .
C7 C 0.2624(2) 0.99321(17) 0.43997(16) 0.0190(5) Uani 1 1 d . . . . .
H7 H 0.277694 1.004888 0.383792 0.023 Uiso 1 1 calc R . . . .
C16 C 0.1215(2) 0.86684(18) 1.00842(15) 0.0193(5) Uani 1 1 d . . . . .
H16 H 0.190162 0.894237 1.036826 0.023 Uiso 1 1 calc R . . . .
C30 C 0.0149(2) 0.56163(18) 0.72394(16) 0.0193(5) Uani 1 1 d . . . . .
H30 H 0.039838 0.599474 0.769015 0.023 Uiso 1 1 calc R . . . .
C26 C 0.0628(2) 0.47325(18) 0.60815(16) 0.0192(5) Uani 1 1 d . . . . .
H26 H 0.120457 0.450371 0.573062 0.023 Uiso 1 1 calc R . . . .
C9 C 0.1445(2) 1.01633(17) 0.55647(16) 0.0214(6) Uani 1 1 d . . . . .
H9 H 0.079400 1.044837 0.580750 0.026 Uiso 1 1 calc R . . . .
C8 C 0.1667(2) 1.03476(17) 0.47450(16) 0.0202(5) Uani 1 1 d . . . . .
H8 H 0.116832 1.075300 0.442591 0.024 Uiso 1 1 calc R . . . .
C28 C -0.1430(2) 0.48317(18) 0.64518(18) 0.0223(6) Uani 1 1 d . . . . .
H28 H -0.226203 0.467392 0.635601 0.027 Uiso 1 1 calc R . . . .
C29 C -0.1064(2) 0.53891(19) 0.70968(17) 0.0231(6) Uani 1 1 d . . . . .
H29 H -0.164492 0.561804 0.744446 0.028 Uiso 1 1 calc R . . . .
C1 C 0.6950(2) 0.76814(18) 0.69557(17) 0.0217(6) Uani 1 1 d . . . . .
H1A H 0.718702 0.785740 0.753132 0.033 Uiso 1 1 calc GR . . . .
H1B H 0.748481 0.796797 0.658020 0.033 Uiso 1 1 calc GR . . . .
H1C H 0.702239 0.704245 0.690471 0.033 Uiso 1 1 calc GR . . . .
C17 C 0.0057(2) 0.88999(19) 1.02737(16) 0.0241(6) Uani 1 1 d . . . . .
H17 H -0.004765 0.933294 1.068685 0.029 Uiso 1 1 calc R . . . .
C19 C -0.0798(2) 0.7889(2) 0.92642(17) 0.0232(6) Uani 1 1 d . . . . .
H19 H -0.149119 0.762600 0.897767 0.028 Uiso 1 1 calc R . . . .
C27 C -0.0585(2) 0.45013(18) 0.59428(18) 0.0233(6) Uani 1 1 d . . . . .
H27 H -0.083637 0.411577 0.549827 0.028 Uiso 1 1 calc R . . . .
C18 C -0.0944(2) 0.8508(2) 0.98682(17) 0.0247(6) Uani 1 1 d . . . . .
H18 H -0.173725 0.866444 1.000591 0.030 Uiso 1 1 calc R . . . .
B1 B 0.4678(2) 0.69524(19) 0.78104(17) 0.0136(5) Uani 1 1 d . . . . .
H1 H 0.552324 0.675259 0.798343 0.016 Uiso 1 1 calc R . . . .


_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
Zn1 Cl1 2.1743(6) . ?
Zn1 N3 2.0387(19) . ?
Zn1 N5 2.037(2) . ?
Zn1 N1 2.0450(19) . ?
N3 N4 1.369(3) . ?
N3 C14 1.344(3) . ?
N6 N5 1.378(3) . ?
N6 C22 1.349(3) . ?
N6 B1 1.546(3) . ?
N5 C24 1.340(3) . ?
N4 C12 1.353(3) . ?
N4 B1 1.546(3) . ?
N2 N1 1.378(3) . ?
N2 C2 1.353(3) . ?
N2 B1 1.537(3) . ?
N1 C4 1.343(3) . ?
C22 C23 1.382(3) . ?
C22 C21 1.494(3) . ?
C23 H23 0.9500 . ?
C23 C24 1.398(3) . ?
C15 C14 1.473(3) . ?
C15 C20 1.390(3) . ?
C15 C16 1.391(3) . ?
C12 C13 1.377(3) . ?
C12 C11 1.485(3) . ?
C14 C13 1.396(3) . ?
C13 H13 0.9500 . ?
C10 H10 0.9500 . ?
C10 C5 1.394(3) . ?
C10 C9 1.383(3) . ?
C25 C24 1.471(3) . ?
C25 C30 1.393(3) . ?
C25 C26 1.386(3) . ?
C6 H6 0.9500 . ?
C6 C5 1.394(3) . ?
C6 C7 1.388(3) . ?
C3 H3 0.9500 . ?
C3 C2 1.369(3) . ?
C3 C4 1.395(3) . ?
C2 C1 1.495(3) . ?
C5 C4 1.472(3) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C20 H20 0.9500 . ?
C20 C19 1.392(3) . ?
C7 H7 0.9500 . ?
C7 C8 1.385(4) . ?
C16 H16 0.9500 . ?
C16 C17 1.383(3) . ?
C30 H30 0.9500 . ?
C30 C29 1.384(3) . ?
C26 H26 0.9500 . ?
C26 C27 1.384(3) . ?
C9 H9 0.9500 . ?
C9 C8 1.390(4) . ?
C8 H8 0.9500 . ?
C28 H28 0.9500 . ?
C28 C29 1.377(4) . ?
C28 C27 1.384(4) . ?
C29 H29 0.9500 . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C17 H17 0.9500 . ?
C17 C18 1.375(4) . ?
C19 H19 0.9500 . ?
C19 C18 1.372(4) . ?
C27 H27 0.9500 . ?
C18 H18 0.9500 . ?
B1 H1 1.0000 . ?

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
N3 Zn1 Cl1 124.53(5) . . ?
N3 Zn1 N1 96.45(8) . . ?
N5 Zn1 Cl1 120.60(6) . . ?
N5 Zn1 N3 88.80(8) . . ?
N5 Zn1 N1 96.09(8) . . ?
N1 Zn1 Cl1 122.26(6) . . ?
N4 N3 Zn1 110.92(14) . . ?
C14 N3 Zn1 142.20(16) . . ?
C14 N3 N4 106.67(18) . . ?
N5 N6 B1 120.07(19) . . ?
C22 N6 N5 109.57(19) . . ?
C22 N6 B1 130.31(19) . . ?
N6 N5 Zn1 111.12(15) . . ?
C24 N5 Zn1 140.70(16) . . ?
C24 N5 N6 106.52(19) . . ?
N3 N4 B1 120.91(18) . . ?
C12 N4 N3 109.97(18) . . ?
C12 N4 B1 129.07(19) . . ?
N1 N2 B1 120.40(18) . . ?
C2 N2 N1 109.74(19) . . ?
C2 N2 B1 129.32(19) . . ?
N2 N1 Zn1 111.28(14) . . ?
C4 N1 Zn1 141.66(16) . . ?
C4 N1 N2 106.35(18) . . ?
N6 C22 C23 108.3(2) . . ?
N6 C22 C21 122.9(2) . . ?
C23 C22 C21 128.8(2) . . ?
C22 C23 H23 127.3 . . ?
C22 C23 C24 105.4(2) . . ?
C24 C23 H23 127.3 . . ?
C20 C15 C14 121.0(2) . . ?
C20 C15 C16 118.9(2) . . ?
C16 C15 C14 120.1(2) . . ?
N4 C12 C13 107.6(2) . . ?
N4 C12 C11 123.2(2) . . ?
C13 C12 C11 129.2(2) . . ?
N3 C14 C15 122.1(2) . . ?
N3 C14 C13 109.6(2) . . ?
C13 C14 C15 128.3(2) . . ?
C12 C13 C14 106.1(2) . . ?
C12 C13 H13 126.9 . . ?
C14 C13 H13 126.9 . . ?
C5 C10 H10 119.9 . . ?
C9 C10 H10 119.9 . . ?
C9 C10 C5 120.2(2) . . ?
C30 C25 C24 120.6(2) . . ?
C26 C25 C24 120.4(2) . . ?
C26 C25 C30 118.8(2) . . ?
C5 C6 H6 119.9 . . ?
C7 C6 H6 119.9 . . ?
C7 C6 C5 120.2(2) . . ?
C2 C3 H3 126.8 . . ?
C2 C3 C4 106.4(2) . . ?
C4 C3 H3 126.8 . . ?
N2 C2 C3 107.9(2) . . ?
N2 C2 C1 123.3(2) . . ?
C3 C2 C1 128.8(2) . . ?
N5 C24 C23 110.2(2) . . ?
N5 C24 C25 122.2(2) . . ?
C23 C24 C25 127.2(2) . . ?
C10 C5 C6 119.1(2) . . ?
C10 C5 C4 121.6(2) . . ?
C6 C5 C4 119.3(2) . . ?
N1 C4 C3 109.6(2) . . ?
N1 C4 C5 125.0(2) . . ?
C3 C4 C5 125.3(2) . . ?
C22 C21 H21A 109.5 . . ?
C22 C21 H21B 109.5 . . ?
C22 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C12 C11 H11A 109.5 . . ?
C12 C11 H11B 109.5 . . ?
C12 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C15 C20 H20 120.0 . . ?
C15 C20 C19 120.1(2) . . ?
C19 C20 H20 120.0 . . ?
C6 C7 H7 119.7 . . ?
C8 C7 C6 120.6(2) . . ?
C8 C7 H7 119.7 . . ?
C15 C16 H16 119.9 . . ?
C17 C16 C15 120.3(2) . . ?
C17 C16 H16 119.9 . . ?
C25 C30 H30 119.7 . . ?
C29 C30 C25 120.6(2) . . ?
C29 C30 H30 119.7 . . ?
C25 C26 H26 119.7 . . ?
C27 C26 C25 120.6(2) . . ?
C27 C26 H26 119.7 . . ?
C10 C9 H9 119.6 . . ?
C10 C9 C8 120.8(2) . . ?
C8 C9 H9 119.6 . . ?
C7 C8 C9 119.1(2) . . ?
C7 C8 H8 120.5 . . ?
C9 C8 H8 120.5 . . ?
C29 C28 H28 120.0 . . ?
C29 C28 C27 120.0(2) . . ?
C27 C28 H28 120.0 . . ?
C30 C29 H29 120.0 . . ?
C28 C29 C30 120.1(2) . . ?
C28 C29 H29 120.0 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C16 C17 H17 119.8 . . ?
C18 C17 C16 120.4(3) . . ?
C18 C17 H17 119.8 . . ?
C20 C19 H19 119.8 . . ?
C18 C19 C20 120.3(2) . . ?
C18 C19 H19 119.8 . . ?
C26 C27 H27 120.0 . . ?
C28 C27 C26 120.0(2) . . ?
C28 C27 H27 120.0 . . ?
C17 C18 H18 120.0 . . ?
C19 C18 C17 120.0(2) . . ?
C19 C18 H18 120.0 . . ?
N6 B1 H1 109.5 . . ?
N4 B1 N6 109.63(19) . . ?
N4 B1 H1 109.5 . . ?
N2 B1 N6 108.61(19) . . ?
N2 B1 N4 110.1(2) . . ?
N2 B1 H1 109.5 . . ?

_olex2_exptl_crystal_mounting_method 
'Mounted on a MicroMount rod with Paratone-N oil.'
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_scc139_0m
_database_code_depnum_ccdc_archive 'CCDC 2015383'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/D0SC03777J 2020
loop_
_audit_author_name
_audit_author_address
'Scott Coste'
;Northwestern University
United States of America
;
_audit_update_record             
;
2020-07-09 deposited with the CCDC.	2020-09-08 downloaded from the CCDC.
;
_audit_creation_date             2019-03-08
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        
'hydrotris(3-phenyl-5-methylpyrazolyl)borate zinc triphenylstannide'
_chemical_formula_moiety         'C48 H43 B1 N6 Sn1 Zn1'
_chemical_formula_sum            'C54 H49 B N6 Sn Zn'
_chemical_formula_weight         976.86
_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 0.0033 0.0016 '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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sn Sn -0.6537 1.4246 '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      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3'
_space_group_name_Hall           '-R 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   12.3859(4)
_cell_length_b                   12.3859(4)
_cell_length_c                   48.7382(18)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     6475.2(5)
_cell_formula_units_Z            6
_cell_measurement_reflns_used    9878
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      29.017
_cell_measurement_theta_min      2.507
_shelx_estimated_absorpt_T_max   0.950
_shelx_estimated_absorpt_T_min   0.607
_exptl_absorpt_coefficient_mu    1.181
_exptl_absorpt_correction_T_max  0.9514
_exptl_absorpt_correction_T_min  0.7101
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1284 before and 0.0554 after correction. The Ratio of minimum to maximum transmission is 0.7464. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.503
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             3000
_exptl_crystal_preparation       
'Synthesized by the reaction of KSnPh3 with TpZnCl.'
_exptl_crystal_recrystallization_method 
'Crystallized from a benzene/hexane layering.'
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.044
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0448
_diffrn_reflns_av_unetI/netI     0.0175
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       66
_diffrn_reflns_limit_l_min       -66
_diffrn_reflns_number            54021
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.189
_diffrn_reflns_theta_min         1.944
_diffrn_ambient_temperature      99.99
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_special_details          ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3378
_reflns_number_total             3891
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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       'SAINT V8.38A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_refine_diff_density_max         2.478
_refine_diff_density_min         -1.618
_refine_diff_density_rms         0.099
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         3891
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0501
_refine_ls_R_factor_gt           0.0422
_refine_ls_restrained_S_all      1.088
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0528P)²+36.8446P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1096
_refine_ls_wR_factor_ref         0.1172
_refine_special_details          
'Refined with a solvent mask due to benzene molecule disordered over a special position.'
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 B1(H1)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C13(H13), C12(H12), C3(H3), C14(H14), C10(H10),
 C9(H9), C15(H15), C16(H16)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C)
;
_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
Sn1 Sn 0.333333 0.666667 0.39468(2) 0.02978(11) Uani 1 3 d S T P . .
Zn1 Zn 0.333333 0.666667 0.44813(2) 0.02188(13) Uani 1 3 d S T P . .
N1 N 0.48693(19) 0.7034(2) 0.47260(4) 0.0209(4) Uani 1 1 d . . . . .
N2 N 0.45410(19) 0.6748(2) 0.49980(4) 0.0210(4) Uani 1 1 d . . . . .
C6 C 0.6584(3) 0.8189(3) 0.42450(5) 0.0274(5) Uani 1 1 d . . . . .
H6 H 0.604468 0.851314 0.427762 0.033 Uiso 1 1 calc R . . . .
C7 C 0.7292(3) 0.8510(3) 0.40066(6) 0.0317(6) Uani 1 1 d . . . . .
H7 H 0.724047 0.905865 0.387806 0.038 Uiso 1 1 calc R . . . .
C5 C 0.6659(3) 0.7397(3) 0.44363(6) 0.0313(6) Uani 1 1 d . . . . .
C2 C 0.5398(3) 0.6585(3) 0.51307(6) 0.0326(6) Uani 1 1 d . . . . .
C4 C 0.5964(3) 0.7073(3) 0.46961(6) 0.0307(6) Uani 1 1 d . . . . .
C8 C 0.8075(3) 0.8031(3) 0.39554(6) 0.0401(7) Uani 1 1 d . . . . .
H8 H 0.855945 0.825514 0.379240 0.048 Uiso 1 1 calc R . . . .
C13 C 0.4956(4) 0.4240(3) 0.37924(7) 0.0471(8) Uani 1 1 d . . . . .
H13 H 0.552977 0.407318 0.388604 0.057 Uiso 1 1 calc R . . . .
C12 C 0.4698(3) 0.5138(3) 0.38915(6) 0.0375(7) Uani 1 1 d . . . . .
H12 H 0.510693 0.558591 0.405304 0.045 Uiso 1 1 calc R . . . .
C11 C 0.3854(3) 0.5402(3) 0.37599(6) 0.0345(6) Uani 1 1 d . . . . .
C3 C 0.6326(3) 0.6793(4) 0.49457(7) 0.0486(10) Uani 1 1 d . . . . .
H3 H 0.706053 0.675413 0.498065 0.058 Uiso 1 1 calc R . . . .
C1 C 0.5306(3) 0.6229(4) 0.54257(6) 0.0411(8) Uani 1 1 d . . . . .
H1A H 0.496038 0.665943 0.553104 0.062 Uiso 1 1 calc GR . . . .
H1B H 0.613753 0.646649 0.549566 0.062 Uiso 1 1 calc GR . . . .
H1C H 0.475975 0.532536 0.544409 0.062 Uiso 1 1 calc GR . . . .
C14 C 0.4365(4) 0.3582(4) 0.35539(8) 0.0531(10) Uani 1 1 d . . . . .
H14 H 0.452072 0.295415 0.348575 0.064 Uiso 1 1 calc R . . . .
C10 C 0.7451(4) 0.6923(4) 0.43819(7) 0.0505(10) Uani 1 1 d . . . . .
H10 H 0.751610 0.638330 0.451102 0.061 Uiso 1 1 calc R . . . .
B1 B 0.333333 0.666667 0.51029(10) 0.0205(8) Uani 1 3 d S T P . .
H1 H 0.333336 0.666667 0.530808 0.025 Uiso 1 3 calc RS T P . .
C9 C 0.8148(4) 0.7233(4) 0.41408(7) 0.0504(9) Uani 1 1 d . . . . .
H9 H 0.867184 0.689302 0.410448 0.061 Uiso 1 1 calc R . . . .
C15 C 0.3563(4) 0.3852(4) 0.34203(7) 0.0547(10) Uani 1 1 d . . . . .
H15 H 0.317551 0.341904 0.325597 0.066 Uiso 1 1 calc R . . . .
C16 C 0.3297(4) 0.4750(4) 0.35191(6) 0.0467(8) Uani 1 1 d . . . . .
H16 H 0.273337 0.491945 0.342195 0.056 Uiso 1 1 calc R . . . .


_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
Sn1 Zn1 2.6052(6) . ?
Sn1 C11 2.170(3) . ?
Sn1 C11 2.170(3) 3_565 ?
Sn1 C11 2.170(3) 2_665 ?
Zn1 N1 2.094(2) 3_565 ?
Zn1 N1 2.094(2) 2_665 ?
Zn1 N1 2.094(2) . ?
N1 N2 1.380(3) . ?
N1 C4 1.340(3) . ?
N2 C2 1.342(3) . ?
N2 B1 1.535(3) . ?
C6 H6 0.9500 . ?
C6 C7 1.388(4) . ?
C6 C5 1.389(4) . ?
C7 H7 0.9500 . ?
C7 C8 1.388(5) . ?
C5 C4 1.470(4) . ?
C5 C10 1.398(4) . ?
C2 C3 1.380(4) . ?
C2 C1 1.491(4) . ?
C4 C3 1.399(4) . ?
C8 H8 0.9500 . ?
C8 C9 1.376(5) . ?
C13 H13 0.9500 . ?
C13 C12 1.389(5) . ?
C13 C14 1.398(5) . ?
C12 H12 0.9500 . ?
C12 C11 1.397(5) . ?
C11 C16 1.396(4) . ?
C3 H3 0.9500 . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C14 H14 0.9500 . ?
C14 C15 1.362(6) . ?
C10 H10 0.9500 . ?
C10 C9 1.393(4) . ?
B1 H1 1.0000 . ?
C9 H9 0.9500 . ?
C15 H15 0.9500 . ?
C15 C16 1.394(6) . ?
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
C11 Sn1 Zn1 114.81(8) 3_565 . ?
C11 Sn1 Zn1 114.81(8) 2_665 . ?
C11 Sn1 Zn1 114.81(8) . . ?
C11 Sn1 C11 103.65(9) 3_565 . ?
C11 Sn1 C11 103.65(9) 2_665 . ?
C11 Sn1 C11 103.65(9) 3_565 2_665 ?
N1 Zn1 Sn1 124.72(6) 2_665 . ?
N1 Zn1 Sn1 124.72(6) 3_565 . ?
N1 Zn1 Sn1 124.72(6) . . ?
N1 Zn1 N1 90.77(8) . 3_565 ?
N1 Zn1 N1 90.76(8) 2_665 3_565 ?
N1 Zn1 N1 90.77(8) 2_665 . ?
N2 N1 Zn1 111.85(15) . . ?
C4 N1 Zn1 137.66(18) . . ?
C4 N1 N2 106.1(2) . . ?
N1 N2 B1 119.3(2) . . ?
C2 N2 N1 110.3(2) . . ?
C2 N2 B1 130.4(2) . . ?
C7 C6 H6 119.7 . . ?
C7 C6 C5 120.6(3) . . ?
C5 C6 H6 119.7 . . ?
C6 C7 H7 119.9 . . ?
C8 C7 C6 120.2(3) . . ?
C8 C7 H7 119.9 . . ?
C6 C5 C4 122.3(3) . . ?
C6 C5 C10 118.5(3) . . ?
C10 C5 C4 119.2(3) . . ?
N2 C2 C3 107.7(2) . . ?
N2 C2 C1 124.1(2) . . ?
C3 C2 C1 128.2(3) . . ?
N1 C4 C5 123.2(2) . . ?
N1 C4 C3 109.9(2) . . ?
C3 C4 C5 126.8(3) . . ?
C7 C8 H8 120.0 . . ?
C9 C8 C7 120.0(3) . . ?
C9 C8 H8 120.0 . . ?
C12 C13 H13 120.2 . . ?
C12 C13 C14 119.5(4) . . ?
C14 C13 H13 120.2 . . ?
C13 C12 H12 119.1 . . ?
C13 C12 C11 121.7(3) . . ?
C11 C12 H12 119.1 . . ?
C12 C11 Sn1 120.2(2) . . ?
C16 C11 Sn1 122.1(3) . . ?
C16 C11 C12 117.5(3) . . ?
C2 C3 C4 105.9(3) . . ?
C2 C3 H3 127.1 . . ?
C4 C3 H3 127.1 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C13 C14 H14 120.4 . . ?
C15 C14 C13 119.2(3) . . ?
C15 C14 H14 120.4 . . ?
C5 C10 H10 119.6 . . ?
C9 C10 C5 120.8(3) . . ?
C9 C10 H10 119.6 . . ?
N2 B1 N2 109.50(18) 3_565 . ?
N2 B1 N2 109.50(18) 2_665 3_565 ?
N2 B1 N2 109.50(18) 2_665 . ?
N2 B1 H1 109.4 2_665 . ?
N2 B1 H1 109.4 3_565 . ?
N2 B1 H1 109.4 . . ?
C8 C9 C10 119.8(3) . . ?
C8 C9 H9 120.1 . . ?
C10 C9 H9 120.1 . . ?
C14 C15 H15 119.2 . . ?
C14 C15 C16 121.5(3) . . ?
C16 C15 H15 119.2 . . ?
C11 C16 H16 119.8 . . ?
C15 C16 C11 120.4(4) . . ?
C15 C16 H16 119.8 . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 0.000 79.6 0.0 ?
2 0.000 0.000 0.355 11.3 0.0 ?
3 0.000 0.000 0.500 167.3 39.7 ?
4 0.000 0.000 0.645 11.3 0.0 ?
5 0.333 0.667 0.167 167.3 39.7 ?
6 0.333 0.667 0.667 79.6 0.0 ?
7 0.333 0.667 0.312 11.3 0.0 ?
8 0.333 0.667 0.021 11.3 0.0 ?
9 0.667 0.333 0.833 167.3 39.6 ?
10 0.667 0.333 0.333 79.6 0.0 ?
11 0.667 0.333 0.979 11.3 0.0 ?
12 0.667 0.333 0.688 11.3 0.0 ?

_olex2_exptl_crystal_mounting_method 
'Mountaed on a MicroMount using Paratone-N oil.'
_olex2_submission_special_instructions 'No special instructions were received'
_chemical_properties_physical    Moisture-sensitive
####################################################################### 
# 
# 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_scc123_0m
_database_code_depnum_ccdc_archive 'CCDC 2015379'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/D0SC03777J 2020
loop_
_audit_author_name
_audit_author_address
'Scott Coste'
;Northwestern University
United States of America
;
_audit_update_record             
;
2020-07-09 deposited with the CCDC.	2020-09-08 downloaded from the CCDC.
;
_audit_creation_date             2019-03-08
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        
'hydrotris(3-phenyl-5-methylpyrazolyl)borate iron triphenylstannide'
_chemical_formula_moiety         'C48 H43 B1 Fe1 N6 Sn1'
_chemical_formula_sum            'C54 H49 B Fe N6 Sn'
_chemical_formula_weight         967.34
_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 0.0033 0.0016 '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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sn Sn -0.6537 1.4246 '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      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3'
_space_group_name_Hall           '-R 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   12.3722(2)
_cell_length_b                   12.3722(2)
_cell_length_c                   48.7964(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     6468.6(2)
_cell_formula_units_Z            6
_cell_measurement_reflns_used    9655
_cell_measurement_temperature    100.
_cell_measurement_theta_max      29.442
_cell_measurement_theta_min      2.530
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.962
_exptl_absorpt_correction_T_max  0.9879
_exptl_absorpt_correction_T_min  0.8782
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0769 before and 0.0615 after correction. The Ratio of minimum to maximum transmission is 0.8890. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.490
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             2976
_exptl_crystal_preparation       
'Synthesized by the reaction of KSnPh3 with TpFeCl.,Magnetic properties'
_exptl_crystal_recrystallization_method 
'Crystallized from a benzene/hexane layering.'
_exptl_crystal_size_max          0.127
_exptl_crystal_size_mid          0.056
_exptl_crystal_size_min          0.025
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0565
_diffrn_reflns_av_unetI/netI     0.0295
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       68
_diffrn_reflns_limit_l_min       -68
_diffrn_reflns_number            37148
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.064
_diffrn_reflns_theta_min         1.252
_diffrn_ambient_temperature      100.01
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_special_details          ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3504
_reflns_number_total             4228
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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       'SAINT V8.38A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_refine_diff_density_max         0.388
_refine_diff_density_min         -0.908
_refine_diff_density_rms         0.064
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         4228
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0303
_refine_ls_restrained_S_all      1.049
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0265P)²+13.7796P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0706
_refine_ls_wR_factor_ref         0.0771
_refine_special_details          
'Refined using a solvent mask due to benzene molecule disordered over a special position.,SQUEEZE'
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 B1(H1)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C13(H13), C7(H7), C12(H12), C8(H8), C16(H16), C14(H14), C3(H3),
 C15(H15), C9(H9), C10(H10)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C)
;
_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
Sn1 Sn 0.666667 0.333333 0.60642(2) 0.02965(7) Uani 1 3 d S T P . .
Fe1 Fe 0.666667 0.333333 0.55111(2) 0.02336(10) Uani 1 3 d S T P . .
N2 N 0.54550(14) 0.32528(13) 0.49958(3) 0.0223(3) Uani 1 1 d . . . . .
N1 N 0.51235(14) 0.29667(14) 0.52668(3) 0.0229(3) Uani 1 1 d . . . . .
C6 C 0.34269(19) 0.18214(18) 0.57485(4) 0.0299(4) Uani 1 1 d . . . . .
H6 H 0.396723 0.149769 0.571457 0.036 Uiso 1 1 calc R . . . .
C5 C 0.33395(19) 0.2608(2) 0.55579(4) 0.0334(4) Uani 1 1 d . . . . .
C13 C 1.0719(2) 0.4957(2) 0.62124(4) 0.0421(5) Uani 1 1 d . . . . .
H13 H 1.145301 0.553507 0.611738 0.051 Uiso 1 1 calc R . . . .
C11 C 0.8457(2) 0.3856(2) 0.62512(4) 0.0331(4) Uani 1 1 d . . . . .
C2 C 0.45963(19) 0.3415(2) 0.48632(4) 0.0341(4) Uani 1 1 d . . . . .
C7 C 0.27302(19) 0.15049(18) 0.59884(4) 0.0334(4) Uani 1 1 d . . . . .
H7 H 0.279300 0.096326 0.611724 0.040 Uiso 1 1 calc R . . . .
C1 C 0.4692(2) 0.3769(3) 0.45673(4) 0.0430(5) Uani 1 1 d . . . . .
H1A H 0.523917 0.467238 0.454831 0.065 Uiso 1 1 calc GR . . . .
H1B H 0.385996 0.352983 0.449679 0.065 Uiso 1 1 calc GR . . . .
H1C H 0.503810 0.333510 0.446299 0.065 Uiso 1 1 calc GR . . . .
C4 C 0.40278(19) 0.2929(2) 0.52968(4) 0.0322(4) Uani 1 1 d . . . . .
C12 C 0.9555(2) 0.4699(2) 0.61174(4) 0.0338(4) Uani 1 1 d . . . . .
H12 H 0.950641 0.510886 0.595713 0.041 Uiso 1 1 calc R . . . .
B1 B 0.666667 0.333333 0.48891(6) 0.0211(6) Uani 1 3 d S T P . .
H1 H 0.666668 0.333333 0.468420 0.025 Uiso 1 3 calc RS T P . .
C8 C 0.1946(2) 0.1976(2) 0.60402(4) 0.0410(5) Uani 1 1 d . . . . .
H8 H 0.146907 0.175577 0.620429 0.049 Uiso 1 1 calc R . . . .
C16 C 0.8572(2) 0.3298(2) 0.64909(4) 0.0441(5) Uani 1 1 d . . . . .
H16 H 0.784332 0.273803 0.659025 0.053 Uiso 1 1 calc R . . . .
C14 C 1.0806(3) 0.4367(3) 0.64466(4) 0.0474(6) Uani 1 1 d . . . . .
H14 H 1.159698 0.452532 0.651052 0.057 Uiso 1 1 calc R . . . .
C3 C 0.3667(2) 0.3206(3) 0.50478(4) 0.0504(7) Uani 1 1 d . . . . .
H3 H 0.293082 0.324279 0.501252 0.060 Uiso 1 1 calc R . . . .
C15 C 0.9734(3) 0.3550(2) 0.65853(4) 0.0507(6) Uani 1 1 d . . . . .
H15 H 0.979069 0.315552 0.674726 0.061 Uiso 1 1 calc R . . . .
C9 C 0.1855(2) 0.2764(3) 0.58538(5) 0.0526(7) Uani 1 1 d . . . . .
H9 H 0.132287 0.309444 0.589028 0.063 Uiso 1 1 calc R . . . .
C10 C 0.2544(2) 0.3075(3) 0.56125(5) 0.0518(7) Uani 1 1 d . . . . .
H10 H 0.247114 0.361124 0.548363 0.062 Uiso 1 1 calc R . . . .


_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
Sn1 Fe1 2.6987(4) . ?
Sn1 C11 2.174(2) 2_655 ?
Sn1 C11 2.174(2) . ?
Sn1 C11 2.174(2) 3_665 ?
Fe1 N1 2.0992(15) . ?
Fe1 N1 2.0992(15) 2_655 ?
Fe1 N1 2.0992(15) 3_665 ?
N2 N1 1.3770(18) . ?
N2 C2 1.342(2) . ?
N2 B1 1.5423(17) . ?
N1 C4 1.341(2) . ?
C6 H6 0.9500 . ?
C6 C5 1.389(3) . ?
C6 C7 1.389(3) . ?
C5 C4 1.472(2) . ?
C5 C10 1.395(3) . ?
C13 H13 0.9500 . ?
C13 C12 1.389(3) . ?
C13 C14 1.389(3) . ?
C11 C12 1.393(3) . ?
C11 C16 1.401(3) . ?
C2 C1 1.496(3) . ?
C2 C3 1.380(3) . ?
C7 H7 0.9500 . ?
C7 C8 1.382(3) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C4 C3 1.395(3) . ?
C12 H12 0.9500 . ?
B1 H1 1.0000 . ?
C8 H8 0.9500 . ?
C8 C9 1.379(3) . ?
C16 H16 0.9500 . ?
C16 C15 1.389(4) . ?
C14 H14 0.9500 . ?
C14 C15 1.377(4) . ?
C3 H3 0.9500 . ?
C15 H15 0.9500 . ?
C9 H9 0.9500 . ?
C9 C10 1.390(3) . ?
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
C11 Sn1 Fe1 114.82(5) 3_665 . ?
C11 Sn1 Fe1 114.82(5) 2_655 . ?
C11 Sn1 Fe1 114.82(5) . . ?
C11 Sn1 C11 103.63(6) 3_665 2_655 ?
C11 Sn1 C11 103.64(6) . 2_655 ?
C11 Sn1 C11 103.63(6) . 3_665 ?
N1 Fe1 Sn1 124.61(4) 3_665 . ?
N1 Fe1 Sn1 124.61(4) . . ?
N1 Fe1 Sn1 124.61(4) 2_655 . ?
N1 Fe1 N1 90.92(5) 2_655 3_665 ?
N1 Fe1 N1 90.92(5) 2_655 . ?
N1 Fe1 N1 90.92(5) 3_665 . ?
N1 N2 B1 119.72(15) . . ?
C2 N2 N1 110.19(14) . . ?
C2 N2 B1 130.09(16) . . ?
N2 N1 Fe1 111.59(10) . . ?
C4 N1 Fe1 137.72(12) . . ?
C4 N1 N2 106.25(14) . . ?
C5 C6 H6 119.8 . . ?
C5 C6 C7 120.48(19) . . ?
C7 C6 H6 119.8 . . ?
C6 C5 C4 122.12(17) . . ?
C6 C5 C10 118.76(18) . . ?
C10 C5 C4 119.09(18) . . ?
C12 C13 H13 120.1 . . ?
C14 C13 H13 120.1 . . ?
C14 C13 C12 119.9(2) . . ?
C12 C11 Sn1 119.54(13) . . ?
C12 C11 C16 117.3(2) . . ?
C16 C11 Sn1 122.86(17) . . ?
N2 C2 C1 123.82(17) . . ?
N2 C2 C3 107.75(16) . . ?
C3 C2 C1 128.42(18) . . ?
C6 C7 H7 119.9 . . ?
C8 C7 C6 120.20(19) . . ?
C8 C7 H7 119.9 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C4 C5 122.82(17) . . ?
N1 C4 C3 109.79(16) . . ?
C3 C4 C5 127.37(18) . . ?
C13 C12 C11 121.71(19) . . ?
C13 C12 H12 119.1 . . ?
C11 C12 H12 119.1 . . ?
N2 B1 N2 109.21(12) 2_655 . ?
N2 B1 N2 109.21(12) 2_655 3_665 ?
N2 B1 N2 109.21(12) 3_665 . ?
N2 B1 H1 109.7 . . ?
N2 B1 H1 109.7 3_665 . ?
N2 B1 H1 109.7 2_655 . ?
C7 C8 H8 120.0 . . ?
C9 C8 C7 119.99(19) . . ?
C9 C8 H8 120.0 . . ?
C11 C16 H16 119.5 . . ?
C15 C16 C11 121.0(2) . . ?
C15 C16 H16 119.5 . . ?
C13 C14 H14 120.3 . . ?
C15 C14 C13 119.4(2) . . ?
C15 C14 H14 120.3 . . ?
C2 C3 C4 106.00(18) . . ?
C2 C3 H3 127.0 . . ?
C4 C3 H3 127.0 . . ?
C16 C15 H15 119.6 . . ?
C14 C15 C16 120.7(2) . . ?
C14 C15 H15 119.6 . . ?
C8 C9 H9 120.0 . . ?
C8 C9 C10 120.0(2) . . ?
C10 C9 H9 120.0 . . ?
C5 C10 H10 119.7 . . ?
C9 C10 C5 120.6(2) . . ?
C9 C10 H10 119.7 . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 0.000 50.1 0.0 ?
2 0.000 0.000 0.355 6.9 0.0 ?
3 0.000 0.000 0.500 132.9 41.2 ?
4 0.000 0.000 0.645 6.9 0.0 ?
5 0.333 0.667 0.167 132.9 41.1 ?
6 0.333 0.667 0.667 50.1 0.0 ?
7 0.333 0.667 0.311 6.9 0.0 ?
8 0.333 0.667 0.022 6.9 0.0 ?
9 0.667 0.333 0.833 132.9 40.7 ?
10 0.667 0.333 0.333 50.1 0.0 ?
11 0.667 0.333 0.978 6.9 0.0 ?
12 0.667 0.333 0.689 6.9 0.0 ?

_olex2_exptl_crystal_mounting_method 
'Mounted on a MicroMount using Paratone-N oil.'
_olex2_submission_special_instructions 'No special instructions were received'
_chemical_properties_physical    Moisture-sensitive
####################################################################### 
# 
# 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_mo_scc142_0m
_database_code_depnum_ccdc_archive 'CCDC 2015380'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/D0SC03777J 2020
loop_
_audit_author_name
_audit_author_address
'Scott Coste'
;Northwestern University
United States of America
;
_audit_update_record             
;
2020-07-09 deposited with the CCDC.	2020-09-08 downloaded from the CCDC.
;
_audit_creation_date             2018-11-27
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        
'hydrotris(3-phenyl-5-methylpyrazolyl)borate magnanese(II) choride'
_chemical_formula_moiety         'C30 H28 B1 Cl1 Mn1 N6'
_chemical_formula_sum            'C30 H28 B Cl Mn N6'
_chemical_formula_weight         573.78
_chemical_absolute_configuration ?
_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 0.0033 0.0016 '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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 '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      trigonal
_space_group_IT_number           161
_space_group_name_H-M_alt        'R 3 c'
_space_group_name_Hall           'R 3 -2"c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-y, -x, z+1/2'
'-x+y, y, z+1/2'
'x, x-y, z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'-y+2/3, -x+1/3, z+5/6'
'-x+y+2/3, y+1/3, z+5/6'
'x+2/3, x-y+1/3, z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-y+1/3, -x+2/3, z+7/6'
'-x+y+1/3, y+2/3, z+7/6'
'x+1/3, x-y+2/3, z+7/6'

_cell_length_a                   12.0230(13)
_cell_length_b                   12.0230(13)
_cell_length_c                   32.558(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     4075.8(10)
_cell_formula_units_Z            6
_cell_measurement_reflns_used    6817
_cell_measurement_temperature    100
_cell_measurement_theta_max      31.353
_cell_measurement_theta_min      3.176
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.616
_exptl_absorpt_correction_T_max  0.4853
_exptl_absorpt_correction_T_min  0.4292
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0780 before and 0.0704 after correction. The Ratio of minimum to maximum transmission is 0.8844. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1782
_exptl_crystal_preparation       
'Synthesized by the reaction of KTP with MnCl2.,Magnetic properties'
_exptl_crystal_recrystallization_method 
'Crystallized from dichloromethane/hexane layering.'
_exptl_crystal_size_max          0.342
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.084
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0713
_diffrn_reflns_av_unetI/netI     0.0382
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            41720
_diffrn_reflns_point_group_measured_fraction_full 0.811
_diffrn_reflns_point_group_measured_fraction_max 0.761
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.213
_diffrn_reflns_theta_min         2.322
_diffrn_ambient_temperature      100.07
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  Triumph
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed tube'
_diffrn_special_details          ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.521
_reflns_Friedel_fraction_full    0.620
_reflns_Friedel_fraction_max     0.523
_reflns_number_gt                2457
_reflns_number_total             2860
_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       'SAINT V8.34A (Bruker, 2017)'
_computing_data_collection       'APEX2 V2017.3 (Bruker, 2017)'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_refine_diff_density_max         0.312
_refine_diff_density_min         -0.358
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details 
;
 Flack x determined using 679 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.014(16)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     119
_refine_ls_number_reflns         2860
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0310
_refine_ls_restrained_S_all      1.061
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0352P)²+0.7709P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0680
_refine_ls_wR_factor_ref         0.0718
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 B1(H1)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C)
;
_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
Mn1 Mn 0.666667 0.333333 0.46560(2) 0.01373(9) Uani 1 3 d S T P . .
Cl1 Cl 0.666667 0.333333 0.39460(2) 0.01660(14) Uani 1 3 d S T P . .
N1 N 0.50244(14) 0.29921(14) 0.50169(4) 0.0154(3) Uani 1 1 d . . . . .
N2 N 0.53317(14) 0.30584(15) 0.54289(4) 0.0159(3) Uani 1 1 d . . . . .
C1 C 0.43225(19) 0.2832(2) 0.61191(5) 0.0250(4) Uani 1 1 d . . . . .
H1A H 0.450970 0.217090 0.621597 0.037 Uiso 1 1 calc GR . . . .
H1B H 0.348172 0.264627 0.622285 0.037 Uiso 1 1 calc GR . . . .
H1C H 0.498515 0.367437 0.621935 0.037 Uiso 1 1 calc GR . . . .
C2 C 0.43090(17) 0.28378(17) 0.56614(5) 0.0177(3) Uani 1 1 d . . . . .
C3 C 0.33132(18) 0.26207(17) 0.54004(5) 0.0187(3) Uani 1 1 d . . . . .
H3 H 0.247514 0.243679 0.547638 0.022 Uiso 1 1 calc R . . . .
C4 C 0.37909(16) 0.27268(16) 0.50013(5) 0.0157(3) Uani 1 1 d . . . . .
C5 C 0.30765(16) 0.25898(16) 0.46177(5) 0.0162(3) Uani 1 1 d . . . . .
C6 C 0.17496(17) 0.21032(18) 0.46329(6) 0.0199(3) Uani 1 1 d . . . . .
H6 H 0.131047 0.183497 0.488803 0.024 Uiso 1 1 calc R . . . .
C7 C 0.10700(17) 0.20097(19) 0.42773(7) 0.0231(4) Uani 1 1 d . . . . .
H7 H 0.017142 0.169137 0.429224 0.028 Uiso 1 1 calc R . . . .
C8 C 0.16865(18) 0.23747(18) 0.39020(6) 0.0231(4) Uani 1 1 d . . . . .
H8 H 0.121389 0.230087 0.365977 0.028 Uiso 1 1 calc R . . . .
C9 C 0.29957(19) 0.2848(2) 0.38818(6) 0.0271(4) Uani 1 1 d . . . . .
H9 H 0.342462 0.309909 0.362459 0.032 Uiso 1 1 calc R . . . .
C10 C 0.36861(18) 0.2957(2) 0.42361(6) 0.0237(4) Uani 1 1 d . . . . .
H10 H 0.458617 0.328691 0.421885 0.028 Uiso 1 1 calc R . . . .
B1 B 0.666667 0.333333 0.55792(11) 0.0162(6) Uani 1 3 d S T P . .
H1 H 0.666664 0.333333 0.588639 0.019 Uiso 1 3 calc RS T P . .


_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
Mn1 Cl1 2.3118(7) . ?
Mn1 N1 2.1534(15) . ?
Mn1 N1 2.1535(15) 3_665 ?
Mn1 N1 2.1535(15) 2_655 ?
N1 N2 1.3830(18) . ?
N1 C4 1.353(2) . ?
N2 C2 1.353(2) . ?
N2 B1 1.5474(18) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C1 C2 1.490(2) . ?
C2 C3 1.382(2) . ?
C3 H3 0.9500 . ?
C3 C4 1.401(2) . ?
C4 C5 1.477(2) . ?
C5 C6 1.399(2) . ?
C5 C10 1.397(2) . ?
C6 H6 0.9500 . ?
C6 C7 1.389(3) . ?
C7 H7 0.9500 . ?
C7 C8 1.382(3) . ?
C8 H8 0.9500 . ?
C8 C9 1.382(3) . ?
C9 H9 0.9500 . ?
C9 C10 1.389(3) . ?
C10 H10 0.9500 . ?
B1 H1 1.0000 . ?

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
N1 Mn1 Cl1 123.07(4) . . ?
N1 Mn1 Cl1 123.07(4) 3_665 . ?
N1 Mn1 Cl1 123.07(4) 2_655 . ?
N1 Mn1 N1 93.06(5) . 3_665 ?
N1 Mn1 N1 93.06(5) 2_655 3_665 ?
N1 Mn1 N1 93.06(5) 2_655 . ?
N2 N1 Mn1 108.98(10) . . ?
C4 N1 Mn1 144.78(11) . . ?
C4 N1 N2 106.24(13) . . ?
N1 N2 B1 122.54(17) . . ?
C2 N2 N1 109.95(13) . . ?
C2 N2 B1 127.51(18) . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
N2 C2 C1 123.34(16) . . ?
N2 C2 C3 108.03(15) . . ?
C3 C2 C1 128.63(17) . . ?
C2 C3 H3 127.0 . . ?
C2 C3 C4 106.04(16) . . ?
C4 C3 H3 127.0 . . ?
N1 C4 C3 109.74(15) . . ?
N1 C4 C5 124.44(14) . . ?
C3 C4 C5 125.81(16) . . ?
C6 C5 C4 119.64(15) . . ?
C10 C5 C4 122.18(15) . . ?
C10 C5 C6 118.16(15) . . ?
C5 C6 H6 119.8 . . ?
C7 C6 C5 120.41(17) . . ?
C7 C6 H6 119.8 . . ?
C6 C7 H7 119.6 . . ?
C8 C7 C6 120.72(17) . . ?
C8 C7 H7 119.6 . . ?
C7 C8 H8 120.2 . . ?
C7 C8 C9 119.51(17) . . ?
C9 C8 H8 120.2 . . ?
C8 C9 H9 119.9 . . ?
C8 C9 C10 120.20(18) . . ?
C10 C9 H9 119.9 . . ?
C5 C10 H10 119.5 . . ?
C9 C10 C5 120.98(17) . . ?
C9 C10 H10 119.5 . . ?
N2 B1 N2 110.48(13) 3_665 . ?
N2 B1 N2 110.48(13) 2_655 3_665 ?
N2 B1 N2 110.48(13) 2_655 . ?
N2 B1 H1 108.4 2_655 . ?
N2 B1 H1 108.4 . . ?
N2 B1 H1 108.4 3_665 . ?

_olex2_exptl_crystal_mounting_method 
'Mounted on a MicroMount rod with Paratone-N oil.'
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_mo_scc115_0m
_database_code_depnum_ccdc_archive 'CCDC 2015382'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/D0SC03777J 2020
loop_
_audit_author_name
_audit_author_address
'Scott Coste'
;Northwestern University
United States of America
;
_audit_update_record             
;
2020-07-09 deposited with the CCDC.	2020-09-08 downloaded from the CCDC.
;
_audit_creation_date             2019-03-08
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        
'hydrotris(3-phenyl-5-methylpyrazolyl)borate manganese triphenylstannide'
_chemical_formula_moiety         'C48 H43 B1 Mn1 N6 Sn1'
_chemical_formula_sum            'C54 H49 B Mn N6 Sn'
_chemical_formula_weight         966.43
_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 0.0033 0.0016 '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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sn Sn -0.6537 1.4246 '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      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3'
_space_group_name_Hall           '-R 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   12.3824(6)
_cell_length_b                   12.3824(6)
_cell_length_c                   49.104(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     6520.2(7)
_cell_formula_units_Z            6
_cell_measurement_reflns_used    9240
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      29.520
_cell_measurement_theta_min      2.522
_shelx_estimated_absorpt_T_max   0.906
_shelx_estimated_absorpt_T_min   0.681
_exptl_absorpt_coefficient_mu    0.912
_exptl_absorpt_correction_T_max  0.9927
_exptl_absorpt_correction_T_min  0.7230
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0593 before and 0.0505 after correction.
The Ratio of minimum to maximum transmission is 0.7283.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.477
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             2970
_exptl_crystal_preparation       
'Prepared from the reaction of KSnPh3 with TpMnCl.,Magnetic properties,Luminescent'
_exptl_crystal_recrystallization_method 
'Crystallized from a benzene/heaxane layering.'
_exptl_crystal_size_max          0.456
_exptl_crystal_size_mid          0.419
_exptl_crystal_size_min          0.11
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0425
_diffrn_reflns_av_unetI/netI     0.0190
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       69
_diffrn_reflns_limit_l_min       -69
_diffrn_reflns_number            55305
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.057
_diffrn_reflns_theta_min         1.944
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_special_details          ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3598
_reflns_number_total             4263
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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       'SAINT V8.38A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_refine_diff_density_max         5.014
_refine_diff_density_min         -1.625
_refine_diff_density_rms         0.119
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         4263
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0653
_refine_ls_R_factor_gt           0.0533
_refine_ls_restrained_S_all      1.048
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0913P)²+44.9508P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1490
_refine_ls_wR_factor_ref         0.1647
_refine_special_details          
'Refined with a solvent mask due to disordered benzene molecule on a special position.,SQUEEZE'
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 B1(H1)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C13(H13), C8(H8), C16(H16), C12(H12), C14(H14), C3(H3),
 C15(H15), C9(H9), C10(H10)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C)
;
_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
Sn1 Sn 0.333333 0.666667 0.44135(2) 0.03032(14) Uani 1 3 d S T P . .
Mn1 Mn 0.333333 0.666667 0.38518(2) 0.02385(18) Uani 1 3 d S T P . .
N2 N 0.3432(2) 0.5545(2) 0.33259(4) 0.0194(4) Uani 1 1 d . . . . .
N1 N 0.3734(2) 0.5497(2) 0.35940(4) 0.0199(4) Uani 1 1 d . . . . .
C6 C 0.4834(3) 0.4940(3) 0.40756(6) 0.0275(6) Uani 1 1 d . . . . .
H6 H 0.514409 0.580156 0.404299 0.033 Uiso 1 1 calc R . . . .
C5 C 0.4072(3) 0.4064(3) 0.38829(6) 0.0307(6) Uani 1 1 d . . . . .
C7 C 0.5143(3) 0.4561(3) 0.43158(6) 0.0314(6) Uani 1 1 d . . . . .
H7 H 0.567272 0.516643 0.444492 0.038 Uiso 1 1 calc R . . . .
C13 C 0.7389(4) 0.8274(4) 0.45469(7) 0.0395(8) Uani 1 1 d . . . . .
H13 H 0.811379 0.884430 0.444882 0.047 Uiso 1 1 calc R . . . .
C2 C 0.3249(3) 0.4517(3) 0.31922(6) 0.0315(7) Uani 1 1 d . . . . .
C11 C 0.5132(3) 0.7187(3) 0.45963(6) 0.0314(6) Uani 1 1 d . . . . .
B1 B 0.333333 0.666667 0.32199(10) 0.0178(8) Uani 1 3 d S T P . .
H1 H 0.333334 0.666664 0.301623 0.021 Uiso 1 3 calc RS T P . .
C8 C 0.4684(4) 0.3309(4) 0.43676(7) 0.0395(8) Uani 1 1 d . . . . .
H8 H 0.490001 0.305574 0.453160 0.047 Uiso 1 1 calc R . . . .
C4 C 0.3757(3) 0.4433(3) 0.36223(6) 0.0295(6) Uani 1 1 d . . . . .
C16 C 0.5266(4) 0.6626(4) 0.48342(7) 0.0417(8) Uani 1 1 d . . . . .
H16 H 0.454904 0.607174 0.493635 0.050 Uiso 1 1 calc R . . . .
C1 C 0.2877(4) 0.4264(3) 0.28991(7) 0.0423(9) Uani 1 1 d . . . . .
H1A H 0.197460 0.391962 0.288291 0.063 Uiso 1 1 calc GR . . . .
H1B H 0.310037 0.366369 0.282686 0.063 Uiso 1 1 calc GR . . . .
H1C H 0.331299 0.504314 0.279537 0.063 Uiso 1 1 calc GR . . . .
C12 C 0.6219(3) 0.8026(3) 0.44597(6) 0.0322(6) Uani 1 1 d . . . . .
H12 H 0.615777 0.844012 0.430264 0.039 Uiso 1 1 calc R . . . .
C14 C 0.7495(4) 0.7683(4) 0.47789(8) 0.0463(10) Uani 1 1 d . . . . .
H14 H 0.828955 0.783682 0.483827 0.056 Uiso 1 1 calc R . . . .
C3 C 0.3455(5) 0.3785(3) 0.33752(7) 0.0461(10) Uani 1 1 d . . . . .
H3 H 0.340199 0.300594 0.333987 0.055 Uiso 1 1 calc R . . . .
C15 C 0.6440(5) 0.6879(4) 0.49204(7) 0.0486(10) Uani 1 1 d . . . . .
H15 H 0.651162 0.648691 0.508026 0.058 Uiso 1 1 calc R . . . .
C9 C 0.3911(5) 0.2427(4) 0.41807(9) 0.0540(12) Uani 1 1 d . . . . .
H9 H 0.358440 0.156602 0.421791 0.065 Uiso 1 1 calc R . . . .
C10 C 0.3607(5) 0.2793(3) 0.39380(8) 0.0522(12) Uani 1 1 d . . . . .
H10 H 0.308272 0.218178 0.380922 0.063 Uiso 1 1 calc R . . . .


_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
Sn1 Mn1 2.7580(8) . ?
Sn1 C11 2.179(3) 2_665 ?
Sn1 C11 2.179(3) 3_565 ?
Sn1 C11 2.179(3) . ?
Mn1 N1 2.160(2) . ?
Mn1 N1 2.160(2) 2_665 ?
Mn1 N1 2.160(2) 3_565 ?
N2 N1 1.378(3) . ?
N2 C2 1.346(4) . ?
N2 B1 1.544(3) . ?
N1 C4 1.339(4) . ?
C6 H6 0.9500 . ?
C6 C5 1.392(4) . ?
C6 C7 1.392(4) . ?
C5 C4 1.476(4) . ?
C5 C10 1.405(5) . ?
C7 H7 0.9500 . ?
C7 C8 1.382(5) . ?
C13 H13 0.9500 . ?
C13 C12 1.390(5) . ?
C13 C14 1.395(6) . ?
C2 C1 1.496(4) . ?
C2 C3 1.388(4) . ?
C11 C16 1.410(4) . ?
C11 C12 1.393(5) . ?
B1 H1 1.0000 . ?
C8 H8 0.9500 . ?
C8 C9 1.381(6) . ?
C4 C3 1.398(4) . ?
C16 H16 0.9500 . ?
C16 C15 1.391(6) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C12 H12 0.9500 . ?
C14 H14 0.9500 . ?
C14 C15 1.371(7) . ?
C3 H3 0.9500 . ?
C15 H15 0.9500 . ?
C9 H9 0.9500 . ?
C9 C10 1.392(5) . ?
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
C11 Sn1 Mn1 114.33(8) 3_565 . ?
C11 Sn1 Mn1 114.33(8) . . ?
C11 Sn1 Mn1 114.33(8) 2_665 . ?
C11 Sn1 C11 104.21(10) 3_565 . ?
C11 Sn1 C11 104.21(10) 2_665 . ?
C11 Sn1 C11 104.21(10) 2_665 3_565 ?
N1 Mn1 Sn1 125.89(6) . . ?
N1 Mn1 Sn1 125.89(6) 2_665 . ?
N1 Mn1 Sn1 125.89(6) 3_565 . ?
N1 Mn1 N1 89.12(8) 3_565 . ?
N1 Mn1 N1 89.12(8) 3_565 2_665 ?
N1 Mn1 N1 89.12(8) . 2_665 ?
N1 N2 B1 120.4(2) . . ?
C2 N2 N1 110.3(2) . . ?
C2 N2 B1 129.3(3) . . ?
N2 N1 Mn1 111.88(16) . . ?
C4 N1 Mn1 136.4(2) . . ?
C4 N1 N2 106.3(2) . . ?
C5 C6 H6 119.8 . . ?
C7 C6 H6 119.8 . . ?
C7 C6 C5 120.4(3) . . ?
C6 C5 C4 121.9(3) . . ?
C6 C5 C10 118.7(3) . . ?
C10 C5 C4 119.3(3) . . ?
C6 C7 H7 119.8 . . ?
C8 C7 C6 120.4(3) . . ?
C8 C7 H7 119.8 . . ?
C12 C13 H13 120.1 . . ?
C12 C13 C14 119.8(4) . . ?
C14 C13 H13 120.1 . . ?
N2 C2 C1 123.8(3) . . ?
N2 C2 C3 107.6(3) . . ?
C3 C2 C1 128.6(3) . . ?
C16 C11 Sn1 123.4(3) . . ?
C12 C11 Sn1 119.0(2) . . ?
C12 C11 C16 117.3(3) . . ?
N2 B1 N2 109.25(19) 3_565 2_665 ?
N2 B1 N2 109.24(19) 3_565 . ?
N2 B1 N2 109.24(19) 2_665 . ?
N2 B1 H1 109.7 3_565 . ?
N2 B1 H1 109.7 2_665 . ?
N2 B1 H1 109.7 . . ?
C7 C8 H8 120.0 . . ?
C9 C8 C7 119.9(3) . . ?
C9 C8 H8 120.0 . . ?
N1 C4 C5 122.3(3) . . ?
N1 C4 C3 110.1(3) . . ?
C3 C4 C5 127.7(3) . . ?
C11 C16 H16 119.7 . . ?
C15 C16 C11 120.6(4) . . ?
C15 C16 H16 119.7 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C13 C12 C11 121.9(3) . . ?
C13 C12 H12 119.1 . . ?
C11 C12 H12 119.1 . . ?
C13 C14 H14 120.3 . . ?
C15 C14 C13 119.3(4) . . ?
C15 C14 H14 120.3 . . ?
C2 C3 C4 105.7(3) . . ?
C2 C3 H3 127.1 . . ?
C4 C3 H3 127.1 . . ?
C16 C15 H15 119.4 . . ?
C14 C15 C16 121.2(3) . . ?
C14 C15 H15 119.4 . . ?
C8 C9 H9 119.8 . . ?
C8 C9 C10 120.3(4) . . ?
C10 C9 H9 119.8 . . ?
C5 C10 H10 119.9 . . ?
C9 C10 C5 120.2(3) . . ?
C9 C10 H10 119.9 . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 0.000 140.8 20.5 ?
2 0.000 0.000 0.146 7.2 0.0 ?
3 0.000 0.000 0.500 45.0 6.2 ?
4 0.000 0.000 0.854 7.2 0.0 ?
5 0.333 0.667 0.667 140.8 20.5 ?
6 0.333 0.667 0.167 45.0 6.2 ?
7 0.333 0.667 0.521 7.2 0.0 ?
8 0.333 0.667 0.812 7.2 0.0 ?
9 0.667 0.333 0.333 140.8 20.5 ?
10 0.667 0.333 0.833 45.0 6.2 ?
11 0.667 0.333 0.188 7.2 0.0 ?
12 0.667 0.333 0.479 7.2 0.0 ?

_olex2_exptl_crystal_mounting_method 
'Mounted on a MicroMount rod with Paratone-N oil'
_olex2_submission_special_instructions 'No special instructions were received'
_chemical_properties_physical    Moisture-sensitive
