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_4341894
_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 F2 Fe2 N10 O2'
_chemical_formula_sum            'C134 H110 B2 F50 Fe2 N10 O6'
_chemical_formula_weight         3039.63
_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                87.114(2)
_cell_angle_beta                 76.7170(10)
_cell_angle_gamma                77.569(2)
_cell_formula_units_Z            1
_cell_length_a                   12.2877(5)
_cell_length_b                   16.8312(7)
_cell_length_c                   17.7318(8)
_cell_measurement_reflns_used    9861
_cell_measurement_temperature    225(2)
_cell_measurement_theta_max      65.13
_cell_measurement_theta_min      3.71
_cell_volume                     3485.4(3)
_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 0.931
_diffrn_measured_fraction_theta_max 0.984
_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  0.0190
_diffrn_reflns_av_unetI/netI     0.0240
_diffrn_reflns_Laue_measured_fraction_full 0.931
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            27225
_diffrn_reflns_point_group_measured_fraction_full 0.931
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         65.236
_diffrn_reflns_theta_min         3.712
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.773
_exptl_absorpt_correction_T_max  0.7526
_exptl_absorpt_correction_T_min  0.5255
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1071 before and 0.0321 after correction.
The Ratio of minimum to maximum transmission is 0.6982.
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    1.448
_exptl_crystal_description       block
_exptl_crystal_F_000             1544
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.827
_refine_diff_density_min         -0.676
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     905
_refine_ls_number_reflns         11734
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.127
_refine_ls_R_factor_all          0.0708
_refine_ls_R_factor_gt           0.0649
_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^)+(0.1308P)^2^+1.4656P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1967
_refine_ls_wR_factor_ref         0.2056
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10478
_reflns_number_total             11734
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5025586_si_002.cif
_cod_data_source_block           compound_4_225k
_cod_depositor_comments
'Adding full bibliography for 4341887--4341894.cif.'
_cod_database_code               4341894
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H12(0.055) H17(0.055) H21(0.055) H24(0.058) H25(0.056) H26(0.057)
 H32(0.063) H33(0.065) H34(0.064) H37(0.066) H53(0.073) H58(0.083) H45A(0.08)
 H45B(0.08) H46(0.068) H48(0.085) H52(0.082) H54(0.087) H55(0.099) H56(0.078)
 H59(0.081) H61A(0.082) H61B(0.082) H63(0.085) H64(0.078) H65A(0.094)
 H65B(0.094) H69(0.091) H72(0.106) H73(0.095) H75(0.119) H83(0.13) H85(0.125)
 H88(0.123) H91(0.106)
 Fixed X: H12(1.1031) H17(1.1324) H21(0.7661) H24(1.2861) H25(1.3913)
 H26(0.927) H32(1.128) H33(1.4575) H34(1.2589) H37(1.0045) H53(1.2945)
 H58(1.1066) H45A(1.1256) H45B(1.1324) H46(1.4933) H48(1.1784) H52(1.4705)
 H54(1.328) H55(1.4559) H56(1.6583) H59(1.2024) H61A(1.3173) H61B(1.284)
 H63(1.4604) H64(1.2156) H65A(1.2047) H65B(1.1429) H69(1.7567) H72(1.1034)
 H73(1.6573) H75(0.9802) H83(1.1848) H85(1.3616) H88(0.8953) H91(1.0043)
 Fixed Y: H12(-0.0535) H17(-0.0931) H21(-0.0078) H24(-0.1663) H25(-0.2458)
 H26(-0.2305) H32(-0.3528) H33(-0.0946) H34(-0.3801) H37(-0.2168) H53(-0.3281)
 H58(-0.4384) H45A(0.2635) H45B(0.3502) H46(0.0074) H48(0.0479) H52(-0.0683)
 H54(-0.0147) H55(0.2553) H56(0.17) H59(0.1732) H61A(0.3675) H61B(0.344)
 H63(0.3622) H64(0.1145) H65A(0.2482) H65B(0.2066) H69(0.2198) H72(0.4114)
 H73(0.3171) H75(0.0717) H83(0.4297) H85(0.3513) H88(0.1451) H91(0.1953)
 Fixed Z: H12(0.1913) H17(0.0467) H21(0.2912) H24(0.2413) H25(0.1144)
 H26(0.2061) H32(0.2502) H33(-0.0656) H34(0.1203) H37(0.0589) H53(0.4161) H58(-
 0.0413) H45A(0.3891) H45B(0.3513) H46(0.2734) H48(0.3855) H52(0.1757)
 H54(0.1092) H55(0.4924) H56(0.2627) H59(0.5661) H61A(0.2916) H61B(0.2159)
 H63(0.1251) H64(0.1414) H65A(0.207) H65B(0.2819) H69(0.1503) H72(0.4828)
 H73(0.0791) H75(0.4319) H83(0.5828) H85(0.5892) H88(0.5437) H91(0.6106)
;
_shelx_res_checksum              20673
_shelx_hkl_checksum              92340
_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'