#------------------------------------------------------------------------------
#$Date: 2020-09-09 04:01:53 +0300 (Wed, 09 Sep 2020) $
#$Revision: 256235 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/90/1559012.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1559012
loop_
_publ_author_name
'Coste, Scott C.'
'Pearson, Tyler J.'
'Altman, Alison B.'
'Klein, Ryan A.'
'Finney, Brian A.'
'Hu, Michael Y.'
'Alp, E. Ercan'
'Vlaisavljevich, Bess'
'Freedman, Danna E.'
_publ_section_title
;
 Orbital energy mismatch engenders high-spin ground states in
 heterobimetallic complexes
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D0SC03777J
_journal_year                    2020
_chemical_formula_moiety         'C48 H43 B1 N6 Sn1 Zn1'
_chemical_formula_sum            'C54 H49 B N6 Sn Zn'
_chemical_formula_weight         976.86
_chemical_name_systematic
'hydrotris(3-phenyl-5-methylpyrazolyl)borate zinc triphenylstannide'
_chemical_properties_physical    Moisture-sensitive
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-03-08
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-07-09 deposited with the CCDC.	2020-09-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   12.3859(4)
_cell_length_b                   12.3859(4)
_cell_length_c                   48.7382(18)
_cell_measurement_reflns_used    9878
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      29.017
_cell_measurement_theta_min      2.507
_cell_volume                     6475.2(4)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_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)'
_diffrn_ambient_temperature      99.99
_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_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_standards_number         0
_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_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.503
_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
_refine_diff_density_max         2.478
_refine_diff_density_min         -1.618
_refine_diff_density_rms         0.099
_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_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0501
_refine_ls_R_factor_gt           0.0422
_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
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3378
_reflns_number_total             3891
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0sc03777j2.cif
_cod_data_source_block           scc139_0m
_cod_original_cell_volume        6475.2(5)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               1559012
_shelx_shelxl_version_number     2016/6
_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.
;
_shelx_estimated_absorpt_t_max   0.950
_shelx_estimated_absorpt_t_min   0.607
_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)
;
_olex2_exptl_crystal_mounting_method
'Mountaed on a MicroMount using Paratone-N oil.'
_olex2_submission_special_instructions 'No special instructions were received'
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'
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 . . . .
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'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/D0SC03777J 2020
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 . . ?
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_
_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 ?
