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_4349442
_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         'C30 H22 Co N6, 2(F6 P)'
_chemical_formula_sum            'C30 H22 Co F12 N6 P2'
_chemical_formula_weight         815.40
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2xa'
_space_group_name_H-M_alt        'P 21 1 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2016-11-24
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.07 svn.r3352 for OlexSys, GUI svn.r5261)
;
_audit_update_record
;
2017-04-12 # Formatted by publCIF

;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.7844(4)
_cell_length_b                   8.7844(4)
_cell_length_c                   20.2850(11)
_cell_measurement_reflns_used    9966
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.01
_cell_measurement_theta_min      2.32
_cell_volume                     1565.31(13)
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0445
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            7674
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.172
_diffrn_reflns_theta_min         1.004
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.757
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6727
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0923 before and 0.0604 after correction.
The Ratio of minimum to maximum transmission is 0.9021.
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    1.730
_exptl_crystal_description       'rect. Prism'
_exptl_crystal_F_000             818
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.604
_refine_diff_density_min         -0.580
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details
;
 Flack x determined using 3519 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.118(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     503
_refine_ls_number_reflns         7674
_refine_ls_number_restraints     61
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0341
_refine_ls_R_factor_gt           0.0337
_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^)+(0.0581P)^2^+0.1620P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0876
_refine_ls_wR_factor_ref         0.0879
_reflns_Friedel_coverage         0.880
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.001
_reflns_number_gt                7618
_reflns_number_total             7674
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            crystal_structures1.cif
_cod_data_source_block           C1
_cod_database_code               4349442
_shelxl_version_number           2012-9
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
N6 \\sim C26 \\sim C30 \\sim C29 \\sim C28 \\sim C27: within 1.7A with sigma of
0.005 and sigma for terminal atoms of 0.01
C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25: within 1.7A with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(F7A) = Uanis(F11A) = Uanis(F9A)
3. Others
 Sof(F9A)=Sof(F7A)=Sof(P2A)=Sof(F10A)=Sof(F11A)=Sof(F8A)=1-FVAR(1)
 Sof(P2B)=Sof(F7B)=Sof(F8B)=Sof(F11B)=Sof(F9B)=Sof(F10B)=FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
 C28(H28), C2(H2), C13(H13), C27(H27), C3(H3), C18(H18), C19(H19), C4(H4),
 C9(H9), C23(H23), C12(H12), C1(H1), C29(H29), C24(H24), C16(H16), C14(H14),
 C7(H7), C8(H8), C22(H22), C15(H15), C30(H30), C17(H17)
;
_shelx_res_checksum              52697
_shelx_hkl_checksum              63324
_olex2_submission_special_instructions 'No special instructions were received'