#------------------------------------------------------------------------------
#$Date: 2020-09-09 04:01:53 +0300 (Wed, 09 Sep 2020) $
#$Revision: 256235 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/90/1559013.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_1559013
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 Fe1 N6 Sn1'
_chemical_formula_sum            'C54 H49 B Fe N6 Sn'
_chemical_formula_weight         967.34
_chemical_name_systematic
'hydrotris(3-phenyl-5-methylpyrazolyl)borate iron 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                   12.3722(2)
_cell_length_b                   12.3722(2)
_cell_length_c                   48.7964(10)
_cell_measurement_reflns_used    9655
_cell_measurement_temperature    100.
_cell_measurement_theta_max      29.442
_cell_measurement_theta_min      2.530
_cell_volume                     6468.6(2)
_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      100.01
_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_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_standards_number         0
_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_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.490
_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
_refine_diff_density_max         0.388
_refine_diff_density_min         -0.908
_refine_diff_density_rms         0.064
_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_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0303
_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
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3504
_reflns_number_total             4228
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0sc03777j2.cif
_cod_data_source_block           scc123_0m
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               1559013
_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.
;
_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)
;
_olex2_exptl_crystal_mounting_method
'Mounted 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 0.666667 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 . . . .
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'
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 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 . . ?
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_
_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 ?
