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_4341890
_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 Br2 Fe2 N10 O2, C4 O'
_chemical_formula_sum            'C128 H92 B2 Br2 F48 Fe2 N10 O3'
_chemical_formula_weight         3023.25
_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                84.820(2)
_cell_angle_beta                 76.042(2)
_cell_angle_gamma                77.842(2)
_cell_formula_units_Z            1
_cell_length_a                   12.4619(5)
_cell_length_b                   17.1585(8)
_cell_length_c                   17.9518(8)
_cell_measurement_reflns_used    9944
_cell_measurement_temperature    225(2)
_cell_measurement_theta_max      65.09
_cell_measurement_theta_min      4.97
_cell_volume                     3638.5(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      224.98
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.926
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0245
_diffrn_reflns_av_unetI/netI     0.0303
_diffrn_reflns_Laue_measured_fraction_full 0.926
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            35141
_diffrn_reflns_point_group_measured_fraction_full 0.926
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         65.086
_diffrn_reflns_theta_min         3.727
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.237
_exptl_absorpt_correction_T_max  0.7526
_exptl_absorpt_correction_T_min  0.5214
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0821 before and 0.0358 after correction.
The Ratio of minimum to maximum transmission is 0.6928.
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    1.380
_exptl_crystal_description       block
_exptl_crystal_F_000             1518
_exptl_crystal_size_max          0.534
_exptl_crystal_size_mid          0.292
_exptl_crystal_size_min          0.267
_refine_diff_density_max         0.837
_refine_diff_density_min         -0.784
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     862
_refine_ls_number_reflns         12189
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0702
_refine_ls_R_factor_gt           0.0663
_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^)+(0.1410P)^2^+2.5350P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2021
_refine_ls_wR_factor_ref         0.2079
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11115
_reflns_number_total             12189
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5025586_si_002.cif
_cod_data_source_block           compound_2_225k
_cod_depositor_comments
'Adding full bibliography for 4341887--4341894.cif.'
_cod_database_code               4341890
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Others
 Fixed Sof: O1(0.5) C5(0.5) C10(0.5) C11(0.5) C13(0.5)
 Fixed Uiso: H16(0.053) H20(0.056) H22(0.058) H25(0.058) H27(0.061) H28(0.058)
 H35(0.068) H39(0.07) H42(0.067) H52(0.075) H77(0.091) H87(0.086) H1(0.099)
 H2(0.071) H3(0.107) H4(0.095) H15(0.071) H40A(0.083) H40B(0.083) H53(0.07)
 H56(0.073) H58(0.088) H62(0.087) H66A(0.088) H66B(0.088) H67A(0.084)
 H67B(0.084) H70(0.084) H71(0.084) H72(0.1) H80(0.089) H82(0.097) H84(0.15)
 H104(0.12) H105(0.132)
 Fixed X: H16(0.8861) H20(0.8527) H22(1.0661) H25(0.6065) H27(0.7105)
 H28(1.2204) H35(0.9883) H39(0.7403) H42(0.5283) H52(0.8783) H77(0.7159)
 H87(0.8879) H1(1.0173) H2(0.8229) H3(1.0997) H4(0.9889) H15(0.7932)
 H40A(0.7152) H40B(0.6836) H53(0.3497) H56(0.5173) H58(0.7766) H62(0.3452)
 H66A(0.8555) H66B(0.7956) H67A(0.8649) H67B(0.8736) H70(0.2485) H71(0.5391)
 H72(0.5477) H80(0.5385) H82(0.666) H84(0.8097) H104(0.894) H105(0.635)
 Fixed Y: H16(0.5605) H20(0.5999) H22(0.7334) H25(0.7522) H27(0.6749)
 H28(0.5099) H35(0.7203) H39(0.8801) H42(0.5995) H52(0.8534) H77(0.8332)
 H87(0.9351) H1(0.4259) H2(0.4507) H3(0.3577) H4(0.315) H15(0.3412)
 H40A(0.1668) H40B(0.144) H53(0.3394) H56(0.499) H58(0.3895) H62(0.1895)
 H66A(0.3032) H66B(0.2606) H67A(0.1614) H67B(0.2467) H70(0.2851) H71(0.1468)
 H72(0.2566) H80(0.5718) H82(0.5171) H84(0.0871) H104(0.1032) H105(0.1645)
 Fixed Z: H16(0.8214) H20(0.9579) H22(0.7923) H25(0.8826) H27(0.7621)
 H28(0.7287) H35(0.9413) H39(0.8773) H42(1.0622) H52(0.7475) H77(0.5831)
 H87(1.0351) H1(0.5744) H2(0.6198) H3(0.4625) H4(0.3953) H15(0.4383)
 H40A(0.7941) H40B(0.7198) H53(0.7433) H56(0.7243) H58(0.8663) H62(0.9281)
 H66A(0.7232) H66B(0.799) H67A(0.6597) H67B(0.6195) H70(0.8534) H71(0.8848)
 H72(0.5186) H80(0.8205) H82(0.8926) H84(0.4324) H104(0.5307) H105(0.4266)
;
_shelx_res_checksum              82171
_shelx_hkl_checksum              94836
_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'