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_7702235
_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
'C50 H54 Co N6, C4 Co O4, 2(C4 H8 O), C3.92 O'
_chemical_formula_sum            'C65.922 H70 Co2 N6 O7'
_chemical_formula_weight         1176.25
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_Int_Tables_number      14
_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                90
_cell_angle_beta                 99.304(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.9171(10)
_cell_length_b                   16.0470(8)
_cell_length_c                   18.9243(9)
_cell_measurement_reflns_used    9224
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.24
_cell_measurement_theta_min      1.64
_cell_volume                     5968.8(5)
_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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100.1
_diffrn_measured_fraction_theta_full 0.9948
_diffrn_measured_fraction_theta_max 0.9948
_diffrn_measurement_device_type  'Bruker Apex2'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0680
_diffrn_reflns_av_unetI/netI     0.0551
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            100311
_diffrn_reflns_theta_full        27.2430
_diffrn_reflns_theta_max         27.24
_diffrn_reflns_theta_min         1.64
_exptl_absorpt_coefficient_mu    0.614
_exptl_absorpt_correction_T_max  0.9700
_exptl_absorpt_correction_T_min  0.8871
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'dark blue'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.3088
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             2473.9219
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.6943
_refine_diff_density_min         -0.8525
_refine_diff_density_rms         0.1330
_refine_ls_d_res_high            0.7763
_refine_ls_d_res_low             12.4304
_refine_ls_goodness_of_fit_ref   1.0506
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    108
_refine_ls_number_parameters     718
_refine_ls_number_reflns         13292
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.0506
_refine_ls_R_factor_all          0.0934
_refine_ls_R_factor_gt           0.0583
_refine_ls_shift/su_max          0.0007
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0693P)^2^+11.8031P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1454
_refine_ls_wR_factor_ref         0.1668
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              25
_reflns_limit_h_min              -25
_reflns_limit_k_max              20
_reflns_limit_k_min              0
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                9224
_reflns_number_total             13292
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c8dt03405b2.cif
_cod_data_source_block           sg783
_cod_database_code               7702235
_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
2. Restrained distances
 C68-O7
 1.4 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C62(H62a,H62b), C61(H61a,H61b), C59(H59a,H59b), C60(H60a,H60b), C57(H57a,
 H57b), C56(H56a,H56b), C58(H58a,H58b), C55(H55a,H55b)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C1(H1), C21(H21), C19(H19), C4(H4), C5(H5), C6(H6), C10(H10),
 C12(H12), C36(H36), C38(H38), C27(H27), C30(H30), C29(H29), C28(H28), C32(H32),
  C45(H45), C47(H47)
3.c Idealised Me refined as rotating group:
 C23(H23a,H23b,H23c), C25(H25a,H25b,H25c), C24(H24a,H24b,H24c), C14(H14a,H14b,
 H14c), C16(H16a,H16b,H16c), C15(H15a,H15b,H15c), C40(H40a,H40b,H40c), C41(H41a,
 H41b,H41c), C35(H35a,H35b,H35c), C49(H49a,H49b,H49c), C50(H50a,H50b,H50c),
 C44(H44a,H44b,H44c)
;
_olex2_submission_original_sample_id sg783
_olex2_submission_special_instructions 'No special instructions were received'