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_4341891
_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, C4 O'
_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     dual
_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                85.809(3)
_cell_angle_beta                 76.479(3)
_cell_angle_gamma                77.825(3)
_cell_formula_units_Z            1
_cell_length_a                   12.2621(8)
_cell_length_b                   16.8244(11)
_cell_length_c                   17.6098(10)
_cell_measurement_reflns_used    9996
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.12
_cell_measurement_theta_min      2.71
_cell_volume                     3451.7(4)
_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    'XM (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.03
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.979
_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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1159
_diffrn_reflns_av_unetI/netI     0.1480
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            57782
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.699
_diffrn_reflns_theta_min         1.190
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.366
_exptl_absorpt_correction_T_max  0.7146
_exptl_absorpt_correction_T_min  0.6253
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1299 before and 0.1074 after correction.
The Ratio of minimum to maximum transmission is 0.8750.
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    1.412
_exptl_crystal_description       block
_exptl_crystal_F_000             1482
_exptl_crystal_size_max          0.352
_exptl_crystal_size_mid          0.145
_exptl_crystal_size_min          0.132
_refine_diff_density_max         1.457
_refine_diff_density_min         -0.835
_refine_diff_density_rms         0.170
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     896
_refine_ls_number_reflns         17460
_refine_ls_number_restraints     1728
_refine_ls_restrained_S_all      0.988
_refine_ls_R_factor_all          0.1662
_refine_ls_R_factor_gt           0.0995
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1651P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2573
_refine_ls_wR_factor_ref         0.2850
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9720
_reflns_number_total             17460
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5025586_si_002.cif
_cod_data_source_block           compound_3_100k
_cod_depositor_comments
'Adding full bibliography for 4341887--4341894.cif.'
_cod_database_code               4341891
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Others
 Fixed Sof: O2(0.5) C1B(0.5) C1C(0.5) C1D(0.5) C1E(0.5)
 Fixed Uiso: H2(0.025) H4(0.028) H6(0.029) H8(0.035) H10(0.046) H12(0.037)
 H14(0.03) H15(0.04) H17(0.049) H18(0.028) H20(0.026) H21(0.033) H30A(0.04)
 H30B(0.04) H32(0.036) H33(0.04) H34(0.042) H35(0.035) H42A(0.054) H42B(0.054)
 H43A(0.075) H43B(0.075) H45(0.059) H46(0.053) H47(0.04) H48(0.036) H49(0.06)
 H52(0.03) H79(0.046) H80(0.045) H81(0.062) H1O(0.057) H1P(0.057) H1Q(0.057)
 H1R(0.057) H0AA(0.057) H1AA(0.057) H2AA(0.057) H3AA(0.057)
 Fixed X: H2(0.6137) H4(0.2754) H6(0.4321) H8(0.5087) H10(0.6101) H12(0.7647)
 H14(0.7922) H15(0.6244) H17(0.7799) H18(0.8983) H20(0.6436) H21(0.972)
 H30A(1.2206) H30B(1.1918) H32(1.0397) H33(0.842) H34(0.7445) H35(0.8471)
 H42A(1.3734) H42B(1.3657) H43A(1.306) H43B(1.357) H45(1.2772) H46(1.1627)
 H47(0.9992) H48(0.673) H49(0.4754) H52(0.7072) H79(1.0207) H80(0.5083)
 H81(0.3925) H1O(1.049) H1P(1.408) H1Q(1.1436) H1R(1.3218) H0AA(1.3468)
 H1AA(1.2234) H2AA(1.0454) H3AA(0.9893)
 Fixed Y: H2(0.4402) H4(0.4884) H6(0.2627) H8(0.2805) H10(0.0619) H12(0.1135)
 H14(0.3257) H15(0.1414) H17(0.1669) H18(0.2459) H20(0.4003) H21(0.4041)
 H30A(0.1728) H30B(0.1403) H32(0.1432) H33(0.1842) H34(0.2833) H35(0.3389)
 H42A(0.2464) H42B(0.1594) H43A(0.267) H43B(0.3125) H45(0.3992) H46(0.5287)
 H47(0.4994) H48(0.5472) H49(0.5723) H52(0.6663) H79(0.5783) H80(0.6906)
 H81(0.6429) H1O(0.2501) H1P(0.1047) H1Q(0.1551) H1R(0.0779) H0AA(0.0911)
 H1AA(0.0771) H2AA(0.1618) H3AA(0.2677)
 Fixed Z: H2(0.1789) H4(0.2802) H6(0.2058) H8(0.0533) H10(-0.0501) H12(0.1144)
 H14(0.2368) H15(0.2477) H17(0.421) H18(0.1123) H20(0.0388) H21(-0.0684) H30A(-
 0.2048) H30B(-0.2794) H32(-0.1174) H33(-0.0769) H34(-0.1525) H35(-0.2626)
 H42A(-0.3908) H42B(-0.3485) H43A(-0.2077) H43B(-0.2869) H45(-0.137) H46(-
 0.1106) H47(-0.2757) H48(-0.6191) H49(-0.5716) H52(-0.4378) H79(-0.1799) H80(-
 0.3896) H81(-0.4556) H1O(-0.491) H1P(-0.4709) H1Q(-0.5818) H1R(-0.5744) H0AA(-
 0.487) H1AA(-0.5614) H2AA(-0.5473) H3AA(-0.4549)
;
_shelx_res_checksum              96161
_shelx_hkl_checksum              15732
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
_olex2_submission_special_instructions 'No special instructions were received'