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_4341888
_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 H48 Fe2 N10 O2'
_chemical_formula_sum            'C134 H112 B2 F48 Fe2 N10 O6'
_chemical_formula_weight         3003.65
_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 2014.02.28 svn.r2899 for OlexSys, GUI svn.r4781)
;
_cell_angle_alpha                86.386(2)
_cell_angle_beta                 75.656(2)
_cell_angle_gamma                76.2440(10)
_cell_formula_units_Z            1
_cell_length_a                   12.3247(6)
_cell_length_b                   16.9752(6)
_cell_length_c                   17.7140(9)
_cell_measurement_reflns_used    9918
_cell_measurement_temperature    225(2)
_cell_measurement_theta_max      64.96
_cell_measurement_theta_min      5.82
_cell_volume                     3487.5(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      225.01
_diffrn_measured_fraction_theta_full 0.917
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0268
_diffrn_reflns_av_unetI/netI     0.0294
_diffrn_reflns_Laue_measured_fraction_full 0.917
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            25794
_diffrn_reflns_point_group_measured_fraction_full 0.917
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         65.026
_diffrn_reflns_theta_min         5.365
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.743
_exptl_absorpt_correction_T_max  0.7526
_exptl_absorpt_correction_T_min  0.4027
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0846 before and 0.0376 after correction.
The Ratio of minimum to maximum transmission is 0.5351.
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    1.430
_exptl_crystal_description       block
_exptl_crystal_F_000             1528
_exptl_crystal_size_max          0.928
_exptl_crystal_size_mid          0.311
_exptl_crystal_size_min          0.254
_refine_diff_density_max         0.828
_refine_diff_density_min         -0.748
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     869
_refine_ls_number_reflns         11581
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0819
_refine_ls_R_factor_gt           0.0741
_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^)+(0.1390P)^2^+2.1540P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2184
_refine_ls_wR_factor_ref         0.2282
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10135
_reflns_number_total             11581
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5025586_si_002.cif
_cod_data_source_block           compound_1_225k
_cod_depositor_comments
'Adding full bibliography for 4341887--4341894.cif.'
_cod_database_code               4341888
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H1D(0.068) H9(0.064) H11(0.065) H12(0.055) H13(0.055) H14(0.054)
 H15(0.058) H18(0.056) H19(0.058) H33(0.064) H42(0.075) H45(0.083) H22(0.055)
 H38(0.073) H44A(0.086) H44B(0.086) H51A(0.101) H51B(0.101) H53(0.079)
 H54(0.09) H55(0.073) H58(0.093) H59(0.096) H62(0.09) H63(0.091) H66(0.096)
 H67(0.093) H69(0.098) H73(0.131) H75(0.109) H78A(0.116) H78B(0.116) H82(0.133)
 H83(0.124) H84(0.096) H86(0.126)
 Fixed X: H1D(0.0507) H9(0.2433) H11(0.4891) H12(0.3757) H13(0.5767)
 H14(0.4053) H15(0.1098) H18(0.7459) H19(0.216) H33(0.3769) H42(0.2139)
 H45(0.3893) H22(0.8067) H38(0.7075) H44A(0.6346) H44B(0.6404) H51A(0.8265)
 H51B(0.7914) H53(1.1677) H54(0.7031) H55(0.9937) H58(0.9703) H59(0.9719)
 H62(0.6816) H63(1.2667) H66(0.8083) H67(0.9576) H69(0.5114) H73(0.4835)
 H75(0.6127) H78A(0.7138) H78B(0.6448) H82(0.7019) H83(0.3995) H84(1.1663)
 H86(0.8826)
 Fixed Y: H1D(0.5844) H9(0.8837) H11(0.7159) H12(0.5912) H13(0.7332)
 H14(0.561) H15(0.7465) H18(0.517) H19(0.673) H33(0.854) H42(0.8326)
 H45(0.9382) H22(0.4908) H38(0.6736) H44A(0.7648) H44B(0.8515) H51A(0.8657)
 H51B(0.8448) H53(0.6593) H54(0.6172) H55(0.5045) H58(0.8619) H59(0.7483)
 H62(0.551) H63(0.7103) H66(0.4859) H67(0.43) H69(0.695) H73(0.5738)
 H75(0.9066) H78A(0.7526) H78B(0.7162) H82(0.9224) H83(0.6469) H84(0.8134)
 H86(0.8411)
 Fixed Z: H1D(1.0631) H9(0.8805) H11(0.9488) H12(0.9512) H13(0.8015)
 H14(0.8006) H15(0.8906) H18(0.7033) H19(0.7629) H33(0.7507) H42(0.5851)
 H45(1.0444) H22(0.555) H38(0.5664) H44A(0.3907) H44B(0.3533) H51A(0.2892)
 H51B(0.2141) H53(0.2511) H54(0.1488) H55(0.2681) H58(0.1207) H59(0.4844)
 H62(0.388) H63(0.1388) H66(0.1182) H67(0.1777) H69(0.6177) H73(0.4397)
 H75(0.4861) H78A(0.2047) H78B(0.2809) H82(0.5833) H83(0.5545) H84(0.0717)
 H86(0.5841)
;
_shelx_res_checksum              50630
_shelx_hkl_checksum              93577
_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'