Orbital energy mismatch engenders high-spin ground states in heterobimetallic complexes
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.; Chemical Science  (2020) –; doi:10.1039/D0SC03777J

data_1559011
_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         'C30 H28 B Cl N6 Zn'
_chemical_formula_sum            'C30 H28 B Cl N6 Zn'
_chemical_formula_weight         584.21
_chemical_name_systematic
'hydrotris(3-phenyl-5-methylpyrazolyl)borate zinc(II) chloride'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-11-27
_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                 94.548(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.0364(8)
_cell_length_b                   15.2242(13)
_cell_length_c                   16.1001(13)
_cell_measurement_reflns_used    4835
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.382
_cell_measurement_theta_min      2.326
_cell_volume                     2696.6(4)
_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)'
_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       '\w and \f scans'
_diffrn_radiation_monochromator  Triumph
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_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_source                   'sealed tube'
_diffrn_standards_number         0
_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 \l/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    1.439
_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
_refine_diff_density_max         0.720
_refine_diff_density_min         -0.685
_refine_diff_density_rms         0.093
_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_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0926
_refine_ls_R_factor_gt           0.0469
_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/[\s^2^(Fo^2^)+(0.0432P)^2^+1.4335P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0900
_refine_ls_wR_factor_ref         0.1048
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5269
_reflns_number_total             7978
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc03777j2.cif
_cod_data_source_block           mo_scc143_0m
_cod_database_code               1559011
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.960
_shelx_estimated_absorpt_t_min   0.713
_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)
;
_shelx_res_checksum              54894
_olex2_exptl_crystal_mounting_method
'Mounted on a MicroMount rod with Paratone-N oil.'
_olex2_submission_special_instructions 'No special instructions were received'