Dinuclear Spin-Crossover Complexes Based on Tetradentate and Bridging Cyanocarbanion Ligands.
Milin, Eric; Belaïd, Sabrina; Patinec, Véronique; Triki, Smail; Chastanet, Guillaume; Marchivie, Mathieu; Inorganic chemistry 55 (2016) 9038–9046; doi:10.1021/acs.inorgchem.6b01542

data_4348723
_publ_section_title
;
 Dinuclear Spin-Crossover Complexes Based on Tetradentate and Bridging
 Cyanocarbanion Ligands.
;
_journal_issue                   17
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9038
_journal_page_last               9046
_journal_paper_doi               10.1021/acs.inorgchem.6b01542
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C58 H40 Fe2 N20, 2(C H4 O)'
_chemical_formula_sum            'C60 H48 Fe2 N20 O2'
_chemical_formula_weight         1192.88
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2015-11-07
_audit_creation_method
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Olex2 1.2
(compiled Sep 16 2015 11:44:03 for OlexSys, GUI svn.r5103)
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_cell_angle_alpha                90
_cell_angle_beta                 102.631(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.6690(10)
_cell_length_b                   24.658(2)
_cell_length_c                   11.5670(10)
_cell_measurement_temperature    100.15
_cell_volume                     2691.0(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
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_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
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_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.3622
_diffrn_detector_type            'Sapphire2, large Be window'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_method       '\w and \f 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  0.1069
_diffrn_reflns_av_unetI/netI     0.0993
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            18396
_diffrn_reflns_point_group_measured_fraction_full 0.997
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_diffrn_reflns_theta_full        25.242
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_diffrn_source                   'Enhance (Mo) X-ray Source'
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_exptl_absorpt_process_details
'CrysAlisPro, Agilent Technologies, Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET) (compiled Aug 4 2014,14:34:23) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.'
_exptl_crystal_colour            red
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_exptl_crystal_description       needle
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_refine_ls_hydrogen_treatment    mixed
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_refine_ls_number_parameters     389
_refine_ls_number_reflns         4864
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0886
_refine_ls_R_factor_gt           0.0582
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_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0499P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1231
_refine_ls_wR_factor_ref         0.1400
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3455
_reflns_number_total             4864
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01542_si_002.cif
_cod_data_source_block           compound2-100K
_cod_database_code               4348723
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.965
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_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B), C13(H13A,H13B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C9(H9), C10(H10), C11(H11), C12(H12),
 C15(H15), C16(H16), C17(H17), C18(H18)
2.c Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C)
2.d Idealised tetrahedral OH refined as rotating group:
 O1(H1A)
;
_olex2_submission_original_sample_id Compound2-100K
_olex2_submission_special_instructions 'No special instructions were received'