Electronic Effects of Ligand Substitution on Spin Crossover in a Series of Diiminoquinonoid-Bridged Fe(II)2 Complexes.
Park, Jesse G.; Jeon, Ie-Rang; Harris, T. David; Inorganic chemistry 54 (2015) 359–369; doi:10.1021/ic5025586

data_4341892
_publ_section_title
;
 Electronic Effects of Ligand Substitution on Spin Crossover in a Series
 of Diiminoquinonoid-Bridged Fe(II)2 Complexes.
;
_journal_issue                   1
_journal_name_full               'Inorganic chemistry'
_journal_page_first              359
_journal_page_last               369
_journal_paper_doi               10.1021/ic5025586
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         '2(C32 H12 B F24), C54 H46 Cl2 Fe2 N10 O2'
_chemical_formula_sum            'C128 H92 B2 Cl2 F48 Fe2 N10 O3'
_chemical_formula_weight         2934.33
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-10-02
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_cell_angle_alpha                84.892(2)
_cell_angle_beta                 76.3140(10)
_cell_angle_gamma                77.330(2)
_cell_formula_units_Z            1
_cell_length_a                   12.3707(5)
_cell_length_b                   17.2025(7)
_cell_length_c                   17.9700(8)
_cell_measurement_reflns_used    9907
_cell_measurement_temperature    225(2)
_cell_measurement_theta_max      65.03
_cell_measurement_theta_min      2.63
_cell_volume                     3622.3(3)
_computing_cell_refinement       'SAINT v8.27A (Bruker, 2012)'
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      224.99
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.932
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0287
_diffrn_reflns_av_unetI/netI     0.0327
_diffrn_reflns_Laue_measured_fraction_full 0.932
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            27985
_diffrn_reflns_point_group_measured_fraction_full 0.932
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         65.183
_diffrn_reflns_theta_min         2.635
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.945
_exptl_absorpt_correction_T_max  0.7526
_exptl_absorpt_correction_T_min  0.4741
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1240 before and 0.0408 after correction.
The Ratio of minimum to maximum transmission is 0.6299.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear greenish brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_description       block
_exptl_crystal_F_000             1482
_exptl_crystal_size_max          0.497
_exptl_crystal_size_mid          0.262
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.915
_refine_diff_density_min         -0.645
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.140
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     827
_refine_ls_number_reflns         12222
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.140
_refine_ls_R_factor_all          0.0804
_refine_ls_R_factor_gt           0.0714
_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^)+(0.1320P)^2^+1.8090P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2155
_refine_ls_wR_factor_ref         0.2265
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10360
_reflns_number_total             12222
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5025586_si_002.cif
_cod_data_source_block           compound_3_225k
_cod_depositor_comments
'Adding full bibliography for 4341887--4341894.cif.'
_cod_database_code               4341892
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H1(0.06) H1A(0.095) H10(0.059) H11(0.071) H12(0.066) H13(0.064)
 H17(0.064) H18(0.079) H20(0.073) H26(0.062) H31(0.074) H44(0.09) H35(0.082)
 H42A(0.088) H42B(0.088) H43(0.107) H45(0.08) H47(0.079) H50(0.089) H53(0.092)
 H54(0.09) H57(0.076) H58(0.09) H59A(0.091) H59B(0.091) H60(0.107) H62A(0.096)
 H62B(0.096) H69(0.096) H71(0.099) H77(0.125) H79(0.106) H80(0.118) H83(0.145)
 H92(0.162)
 Fixed X: H1(-0.1439) H1A(-0.2882) H10(-0.111) H11(-0.01) H12(-0.2894)
 H13(0.0674) H17(-0.3947) H18(-0.1259) H20(-0.2621) H26(0.2241) H31(-0.4705)
 H44(-0.1101) H35(0.2043) H42A(0.3135) H42B(0.2805) H43(-0.0218) H45(0.1748)
 H47(0.6508) H50(0.2204) H53(0.75) H54(0.4644) H57(0.4824) H58(0.4581)
 H59A(0.1224) H59B(0.1303) H60(0.4517) H62A(0.1987) H62B(0.1396) H69(0.6524)
 H71(0.3312) H77(0.1033) H79(0.0075) H80(-0.105) H83(0.3626) H92(0.1875)
 Fixed Y: H1(0.0974) H1A(0.3328) H10(0.0587) H11(0.2163) H12(0.1727)
 H13(0.2311) H17(0.2494) H18(0.3518) H20(0.3784) H26(0.0105) H31(0.0968)
 H44(0.4304) H35(0.16) H42A(0.3568) H42B(0.333) H43(0.0743) H45(0.049)
 H47(0.1597) H50(0.1105) H53(0.2123) H54(-0.0697) H57(0.0018) H58(0.3519)
 H59A(0.2548) H59B(0.3396) H60(0.2446) H62A(0.2403) H62B(0.1978) H69(0.3076)
 H71(-0.0155) H77(0.4016) H79(0.1863) H80(0.143) H83(0.3398) H92(0.417)
 Fixed Z: H1(0.9574) H1A(0.584) H10(0.8192) H11(0.9414) H12(0.7613)
 H13(0.7925) H17(0.8824) H18(0.7492) H20(0.8783) H26(0.7224) H31(1.0612)
 H44(1.0371) H35(0.561) H42A(0.2789) H42B(0.2055) H43(0.4266) H45(0.382)
 H47(0.2571) H50(0.135) H53(0.1461) H54(0.1787) H57(0.2764) H58(0.1155)
 H59A(0.3809) H59B(0.3403) H60(0.4812) H62A(0.2022) H62B(0.2779) H69(0.0725)
 H71(0.1086) H77(0.4674) H79(0.6043) H80(0.5391) H83(0.5721) H92(0.5648)
;
_shelx_res_checksum              43036
_shelx_hkl_checksum              81084
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
_olex2_computing_structure_solution_long 'ShelXS (Sheldrick, 2008)'
_olex2_submission_special_instructions 'No special instructions were received'