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_7702233
_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_absolute_configuration unk
_chemical_formula_moiety         '2(C30 H27 Co2 N3 O5)'
_chemical_formula_sum            'C60 H54 Co4 N6 O10'
_chemical_formula_weight         1254.86
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_Int_Tables_number      4
_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                 100.813(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.3616(10)
_cell_length_b                   11.6941(11)
_cell_length_c                   23.226(2)
_cell_measurement_reflns_used    6131
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      50.21
_cell_measurement_theta_min      1.79
_cell_volume                     2764.3(4)
_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(2)
_diffrn_measured_fraction_theta_full 0.9412
_diffrn_measured_fraction_theta_max 0.9412
_diffrn_measurement_device_type  'Bruker Apex2'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0956
_diffrn_reflns_av_unetI/netI     0.1143
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            47439
_diffrn_reflns_theta_full        23.9996
_diffrn_reflns_theta_max         24.00
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    1.245
_exptl_absorpt_correction_T_max  0.9636
_exptl_absorpt_correction_T_min  0.7889
_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    1.5075
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1291.3378
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.5360
_refine_diff_density_min         -0.9623
_refine_diff_density_rms         0.1387
_refine_ls_abs_structure_details
'Flack, H. D. (1983). Acta Cryst. A39, 876-881.'
_refine_ls_abs_structure_Flack   -0.030(18)
_refine_ls_d_res_high            0.8737
_refine_ls_d_res_low             11.4067
_refine_ls_goodness_of_fit_ref   1.0342
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    84
_refine_ls_number_parameters     733
_refine_ls_number_reflns         8141
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.0342
_refine_ls_R_factor_all          0.0878
_refine_ls_R_factor_gt           0.0491
_refine_ls_shift/su_max          0.0008
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0441P)^2^+0.4218P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0893
_refine_ls_wR_factor_ref         0.1019
_reflns_Friedel_coverage         0.891
_reflns_limit_h_max              11
_reflns_limit_h_min              -11
_reflns_limit_k_max              12
_reflns_limit_k_min              -13
_reflns_limit_l_max              26
_reflns_limit_l_min              -26
_reflns_number_gt                5868
_reflns_number_total             8141
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c8dt03405b2.cif
_cod_data_source_block           sg780
_cod_original_cell_volume        2764.3(5)
_cod_original_sg_symbol_Hall     ' P 2yb'
_cod_database_code               7702233
_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:
 C16(H16), C17(H17), C20(H20), C22(H22), C12(H12), C13(H13), C14(H14),
 C29(H29), C31(H31), C41(H41), C37(H37), C38(H38), C39(H39), C42(H42), C45(H45),
  C47(H47), C54(H54), C56(H56)
2.b Idealised Me refined as rotating group:
 C33(H33a,H33b,H33c), C26(H26a,H26b,H26c), C24(H24a,H24b,H24c), C25(H25a,H25b,
 H25c), C35(H35a,H35b,H35c), C34(H34a,H34b,H34c), C49(H49a,H49b,H49c), C50(H50a,
 H50b,H50c), C51(H51a,H51b,H51c), C58(H58a,H58b,H58c), C60(H60a,H60b,H60c),
 C59(H59a,H59b,H59c)
;
_olex2_submission_original_sample_id sg780
_olex2_submission_special_instructions 'No special instructions were received'