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_7702234
_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         '2(C35 H33 Co2 N3 O6), 2(C4 H10 O)'
_chemical_formula_sum            'C78 H86 Co4 N6 O14'
_chemical_formula_weight         1567.32
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_symmetry_Int_Tables_number      13
_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                 90.683(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.268(2)
_cell_length_b                   18.2285(17)
_cell_length_c                   21.168(2)
_cell_measurement_reflns_used    9952
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.48
_cell_measurement_theta_min      2.23
_cell_volume                     7820.1(13)
_computing_cell_refinement       'SAINT V8.30C (?, 2016)'
_computing_data_reduction        'SAINT V8.30C (?, 2016)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.1
_diffrn_measured_fraction_theta_full 0.9445
_diffrn_measured_fraction_theta_max 0.9445
_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  0.1091
_diffrn_reflns_av_unetI/netI     0.1700
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            102356
_diffrn_reflns_theta_full        29.5743
_diffrn_reflns_theta_max         29.57
_diffrn_reflns_theta_min         1.12
_exptl_absorpt_coefficient_mu    0.898
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5605
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.1111 before and 0.0826 after correction. The Ratio of minimum to maximum transmission is 0.7512. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            'dark violet'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.3311
_exptl_crystal_description       prism
_exptl_crystal_F_000             3271.0277
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         6.0305
_refine_diff_density_min         -2.8258
_refine_diff_density_rms         0.4006
_refine_ls_d_res_high            0.7200
_refine_ls_d_res_low             18.2285
_refine_ls_goodness_of_fit_ref   1.2155
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    128
_refine_ls_number_parameters     939
_refine_ls_number_reflns         20738
_refine_ls_number_restraints     82
_refine_ls_restrained_S_all      1.2130
_refine_ls_R_factor_all          0.2285
_refine_ls_R_factor_gt           0.1360
_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^)+(0.2P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3441
_refine_ls_wR_factor_ref         0.3922
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              20
_reflns_limit_h_min              -28
_reflns_limit_k_max              25
_reflns_limit_k_min              0
_reflns_limit_l_max              29
_reflns_limit_l_min              -19
_reflns_number_gt                10438
_reflns_number_total             20738
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c8dt03405b2.cif
_cod_data_source_block           sg753_p71a_p2ovrn_s
_cod_original_cell_volume        7820.3(13)
_cod_original_sg_symbol_Hall     '-P 2yc (x-z,y,z)'
_cod_database_code               7702234
_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
 C01B-C02P \\sim C01B-C02R \\sim C01B-C02U \\sim C02P-C02R \\sim C02P-C02U
\\sim C02R-C02U
 with sigma of 0.04
 C02K-C01B \\sim C02K-C02P \\sim C02K-C02R \\sim C02K-C02U
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C02R \\sim C02U \\sim C02P: within 2A with sigma of 0.005 and sigma for
terminal atoms of 0.01
C01I \\sim C01J \\sim C01T \\sim C01V \\sim C01G \\sim C00Z: within 2A with
sigma of 0.005 and sigma for terminal atoms of 0.01
N00C \\sim N00E: within 2A with sigma of 0.005 and sigma for terminal atoms of
0.01
C02R \\sim C02K \\sim C02P \\sim C02U \\sim C01B: within 2A with sigma of 0.005
and sigma for terminal atoms of 0.01
Uanis(N00C) \\sim Ueq, Uanis(N00E) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
4.a Secondary CH2 refined with riding coordinates:
 C01X(H01m,H01q), C020(H6aa,H), C021(H3aa,Ha), C02A(H8aa,Hf)
4.b Aromatic/amide H refined with riding coordinates:
 C00R(H00R), C00W(H00W), C010(H010), C013(H013), C014(H014), C016(H016),
 C017(H017), C01A(H01A), C01C(H01g), C01D(H01D), C01E(H01E), C01H(H01H),
 C01J(H01J), C01N(H01N), C01O(H01O), C01P(H01P), C01V(H01V), C01Y(H01Y)
4.c Idealised Me refined as rotating group:
 C01R(H01i,H01k,H01l), C01Z(H01b,H01c,H01f), C022(H7aa,Hb,Hc), C024(H02a,H02b,
 H02c), C027(H4aa,Hd,He), C02B(H02v,H02w,H02x), C02C(H02y,Hg,Hh), C02E(H5aa,Hi,
 Hj), C02F(H02z,Hk,Hl), C02J(H02,Hm,Hn), C02L(H02d,H02e,H02f), C02M(H02g,H02h,
 H02i), C02N(H9aa,Ho,Hp), C02O(H02j,H02k,H02l), C02P(H0aa,Hq,Hr), C02Q(H02m,
 H02n,H02o), C02R(H1aa,Hs,Ht), C02S(H02p,H02q,H02r), C02T(H02s,H02t,H02u),
 C02U(H2aa,Hu,Hv)
;
_olex2_submission_original_sample_id sg753
_olex2_submission_special_instructions 'No special instructions were received'