Synthesis, Characterization, and DFT Analysis of Bis-Terpyridyl-Based Molecular Cobalt Complexes.
Aroua, Safwan; Todorova, Tanya K.; Hommes, Paul; Chamoreau, Lise-Marie; Reissig, Hans-Ulrich; Mougel, Victor; Fontecave, Marc; Inorganic chemistry 56 (2017) 5930–5940; doi:10.1021/acs.inorgchem.7b00595

data_4349444
_publ_section_title
;
 Synthesis, Characterization, and DFT Analysis of Bis-Terpyridyl-Based
 Molecular Cobalt Complexes.
;
_journal_issue                   10
_journal_name_full               'Inorganic chemistry'
_journal_page_first              5930
_journal_page_last               5940
_journal_paper_doi               10.1021/acs.inorgchem.7b00595
_journal_volume                  56
_journal_year                    2017
_chemical_formula_moiety         'C46 H30 Co N6, C3 H6 O, 2(F6 P)'
_chemical_formula_sum            'C49 H36 Co F12 N6 O P2'
_chemical_formula_weight         1073.71
_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_Hall           'I -4'
_space_group_name_H-M_alt        'I -4'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2016-09-09
_audit_creation_method
;
Olex2 1.2
(compiled 2016.08.25 svn.r3337 for OlexSys, GUI svn.r5221)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   29.201(3)
_cell_length_b                   29.201(3)
_cell_length_c                   11.2474(10)
_cell_measurement_reflns_used    9892
_cell_measurement_temperature    108(2)
_cell_measurement_theta_max      20.75
_cell_measurement_theta_min      2.39
_cell_volume                     9590.6(16)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      108.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.999
_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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1528
_diffrn_reflns_av_unetI/netI     0.1016
_diffrn_reflns_Laue_measured_fraction_full 0.967
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            63682
_diffrn_reflns_point_group_measured_fraction_full 0.967
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.680
_diffrn_reflns_theta_min         2.205
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.516
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5295
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1114 before and 0.0909 after correction.
The Ratio of minimum to maximum transmission is 0.7104.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear dark brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.487
_exptl_crystal_description       plate
_exptl_crystal_F_000             4360
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.618
_refine_diff_density_min         -0.940
_refine_diff_density_rms         0.097
_refine_ls_abs_structure_details
;
 Refined as a perfect inversion twin.
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     642
_refine_ls_number_reflns         9114
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.1215
_refine_ls_R_factor_gt           0.0918
_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^)+127.9633P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1802
_refine_ls_wR_factor_ref         0.1942
_reflns_Friedel_coverage         0.896
_reflns_Friedel_fraction_full    0.966
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                6991
_reflns_number_total             9114
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            crystal_structures1.cif
_cod_data_source_block           C4
_cod_original_cell_volume        9590.8(19)
_cod_database_code               4349444
_shelxl_version_number           2012-9
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C16) \\sim Ueq, Uanis(C9) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C46(H46), C8(H8), C23(H23), C39(H39), C29(H29), C31(H31), C26(H26), C12(H12),
 C28(H28), C34(H34), C11(H11), C35(H35), C42(H42), C3(H3), C27(H27), C13(H13),
 C16(H16), C41(H41), C19(H19), C18(H18), C4(H4), C20(H20), C21(H21), C6(H6),
 C5(H5), C44(H44), C1(H1), C36(H36), C43(H43), C24(H24)
3.b Idealised Me refined as rotating group:
 C49(H49A,H49B,H49C), C47(H47A,H47B,H47C)
;
_shelx_res_checksum              13314
_shelx_hkl_checksum              10439
_shelx_fab_checksum              44775
_olex2_submission_special_instructions 'No special instructions were received'