Reactions of dicobalt octacarbonyl with dinucleating and mononucleating bis(imino)pyridine ligands.
Hollingsworth, Ryan L.; Beattie, Jeffrey W.; Grass, Amanda; Martin, Philip D.; Groysman, Stanislav; Lord, Richard L.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 15353–15363; doi:10.1039/c8dt03405b

data_7702231
_publ_section_title
;
 Reactions of dicobalt octacarbonyl with dinucleating and mononucleating
 bis(imino)pyridine ligands.
;
_journal_issue                   43
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15353
_journal_page_last               15363
_journal_paper_doi               10.1039/c8dt03405b
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C68 H78 Co2 N10 O2, 2(C4 Co O4)'
_chemical_formula_sum            'C76 H78 Co4 N10 O10'
_chemical_formula_weight         1527.26
_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_Int_Tables_number      2
_atom_sites_solution_primary     direct
_audit_creation_date             2018-09-25
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-09-25 deposited with the CCDC.
2018-09-27 downloaded from the CCDC.
;
_cell_angle_alpha                101.991(7)
_cell_angle_beta                 90.788(10)
_cell_angle_gamma                118.813(5)
_cell_formula_units_Z            2
_cell_length_a                   14.541(6)
_cell_length_b                   14.765(6)
_cell_length_c                   20.123(6)
_cell_measurement_reflns_used    9478
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.60
_cell_measurement_theta_min      1.61
_cell_volume                     3670(2)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.9845
_diffrn_measured_fraction_theta_max 0.9845
_diffrn_measurement_device_type  'Bruker Apex'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0703
_diffrn_reflns_av_unetI/netI     0.0629
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            60046
_diffrn_reflns_theta_full        25.6010
_diffrn_reflns_theta_max         25.60
_diffrn_reflns_theta_min         1.61
_exptl_absorpt_coefficient_mu    0.953
_exptl_absorpt_correction_T_max  0.9041
_exptl_absorpt_correction_T_min  0.7696
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'dark violet'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.3819
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prisms
_exptl_crystal_F_000             1587.2725
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.6692
_refine_diff_density_min         -0.4961
_refine_diff_density_rms         0.1098
_refine_ls_d_res_high            0.8224
_refine_ls_d_res_low             12.6278
_refine_ls_goodness_of_fit_ref   1.0188
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    116
_refine_ls_number_parameters     921
_refine_ls_number_reflns         13592
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0188
_refine_ls_R_factor_all          0.0779
_refine_ls_R_factor_gt           0.0493
_refine_ls_shift/su_max          0.0004
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0580P)^2^+2.5269P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1146
_refine_ls_wR_factor_ref         0.1335
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              17
_reflns_limit_h_min              -17
_reflns_limit_k_max              17
_reflns_limit_k_min              -17
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                9478
_reflns_number_total             13592
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c8dt03405b2.cif
_cod_data_source_block           sg917a
_cod_database_code               7702231
_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.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C7(H7), C9(H9), C15(H15), C16(H16), C17(H17), C19(H19), C24(H24),
 C27(H27), C28(H28), C29(H29), C30(H30), C37(H37), C38(H38), C42(H42), C49(H49),
  C50(H50), C58(H58)
2.b Idealised Me refined as rotating group:
 C22(H22a,H22b,H22c), C34(H34a,H34b,H34c), C36(H36a,H36b,H36c), C44(H44a,H44b,
 H44c), C48(H48a,H48b,H48c), C55(H55a,H55b,H55c), C62(H62a,H62b,H62c), C65(H65a,
 H65b,H65c), C69(H69a,H69b,H69c), C80(H80a,H80b,H80c), C82(H82a,H82b,H82c),
 C79(H79a,H79b,H79c), C83(H83a,H83b,H83c), C78(H78a,H78b,H78c), C75(H75a,H75b,
 H75c), C76(H76a,H76b,H76c), C77(H77a,H77b,H77c), C84(H84a,H84b,H84c), C88(H88a,
 H88b,H88c), C89(H89a,H89b,H89c)
;
_olex2_submission_original_sample_id sg917a
_olex2_submission_special_instructions 'No special instructions were received'