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_7702232
_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         'C70 H66 Co4 N6 O12, 2(C4 H9 O)'
_chemical_formula_sum            'C78 H84 Co4 N6 O14'
_chemical_formula_weight         1565.30
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_Int_Tables_number      15
_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                90
_cell_angle_beta                 102.7044(15)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.960(3)
_cell_length_b                   10.0567(12)
_cell_length_c                   30.999(4)
_cell_measurement_reflns_used    8005
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.33
_cell_measurement_theta_min      2.19
_cell_volume                     7590.7(16)
_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      173.15
_diffrn_measured_fraction_theta_full 0.9970
_diffrn_measured_fraction_theta_max 0.9970
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0635
_diffrn_reflns_av_unetI/netI     0.0586
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            30048
_diffrn_reflns_theta_full        25.3515
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         1.35
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.926
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6594
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0674 before and 0.0599 after correction.
The Ratio of minimum to maximum transmission is 0.8849.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.3696
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       chunk
_exptl_crystal_F_000             3263.0282
_exptl_crystal_size_max          0.289
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.131
_refine_diff_density_max         0.8882
_refine_diff_density_min         -0.4234
_refine_diff_density_rms         0.1069
_refine_ls_d_res_high            0.8300
_refine_ls_d_res_low             15.1199
_refine_ls_goodness_of_fit_ref   1.0157
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    63
_refine_ls_number_parameters     470
_refine_ls_number_reflns         6934
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0157
_refine_ls_R_factor_all          0.0740
_refine_ls_R_factor_gt           0.0481
_refine_ls_shift/su_max          0.0005
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0486P)^2^+16.7864P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1096
_refine_ls_wR_factor_ref         0.1264
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              29
_reflns_limit_h_min              -30
_reflns_limit_k_max              12
_reflns_limit_k_min              0
_reflns_limit_l_max              37
_reflns_limit_l_min              0
_reflns_number_gt                4873
_reflns_number_total             6934
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c8dt03405b2.cif
_cod_data_source_block           sg817d
_cod_original_cell_volume        7590.6(16)
_cod_database_code               7702232
_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.a Secondary CH2 refined with riding coordinates:
 C51(H51a,H51b)
2.b Aromatic/amide H refined with riding coordinates:
 C35(H35), C13(H13), C9(H9), C11(H11), C15(H15), C5(H5), C8(H8), C28(H28),
 C30(H30), C7(H7)
2.c Idealised Me refined as rotating group:
 C25(H25a,H25b,H25c), C34(H34a,H34b,H34c), C24(H24a,H24b,H24c), C26(H26a,H26b,
 H26c), C22(H22a,H22b,H22c), C33(H33a,H33b,H33c), C21(H21a,H21b,H21c), C32(H32a,
 H32b,H32c), C38(H38a,H38b,H38c), C50(H50a,H50b,H50c)
;
_olex2_submission_original_sample_id sg817d
_olex2_submission_special_instructions 'No special instructions were received'