Synthesis and crystal structure of bis{2-((E)-((4-((E)-1-(methoxyimino)ethyl)phenyl)imino)methyl) phenolato-κ2 N,O}cobalt(II) — ethanol (1/1), C34H36CoN4O5
Yang, Yu-Hua; Wei, Zhi-Li; Li, Yi-Zheng; Zhao, Ji-Xing; Dong, Wen-Kui; Zeitschrift für Kristallographie - New Crystal Structures 234 (2019) 379–381; doi:10.1515/ncrs-2017-0413

data_8105652
_publ_section_title
;
 Synthesis and crystal structure of
 bis{2-((E)-((4-((E)-1-(methoxyimino)ethyl)phenyl)imino)methyl)
 phenolato-\k2 N,O}cobalt(II) --- ethanol (1/1), C34H36CoN4O5
;
_journal_issue                   3
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              379
_journal_page_last               381
_journal_paper_doi               10.1515/ncrs-2017-0413
_journal_volume                  234
_journal_year                    2019
_chemical_formula_moiety         'C32 H30 Co N4 O4, C2 H6 O'
_chemical_formula_sum            'C34 H36 Co N4 O5'
_chemical_formula_weight         639.60
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                99.054(2)
_cell_angle_beta                 95.727(2)
_cell_angle_gamma                92.477(2)
_cell_formula_units_Z            2
_cell_length_a                   8.7040(5)
_cell_length_b                   12.7375(9)
_cell_length_c                   14.2626(9)
_cell_measurement_reflns_used    3535
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.52
_cell_measurement_theta_min      2.35
_cell_volume                     1550.96(17)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS-1997 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0305
_diffrn_reflns_av_unetI/netI     0.0699
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9989
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.500
_diffrn_reflns_theta_min         2.348
_exptl_absorpt_coefficient_mu    0.601
_exptl_crystal_density_diffrn    1.370
_exptl_crystal_description
;
;
_exptl_crystal_F_000             670
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.656
_refine_diff_density_min         -0.367
_refine_diff_density_rms         0.067
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         6366
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0886
_refine_ls_R_factor_gt           0.0554
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0504P)^2^+1.5733P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1211
_refine_ls_wR_factor_ref         0.1369
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4614
_reflns_number_total             6366
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2017-0413_suppl.cif
_cod_data_source_block           1
_cod_database_code               8105652
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O5A-C33
 1.43 with sigma of 0.01
 O5-C33
 1.43 with sigma of 0.01
 C33-C34A
 1.54 with sigma of 0.01
 C33-C34
 1.54 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(O5A) \\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C34A)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(H33C)=Sof(H33D)=Sof(C34A)=Sof(H34A)=Sof(H34B)=Sof(H34C)=Sof(O5A)=
 Sof(H5AA)=1-FVAR(1)
 Sof(H33B)=Sof(H33A)=Sof(O5)=Sof(H5A)=Sof(C34)=Sof(H34D)=Sof(H34E)=Sof(H34F)=
 FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C33(H33B,H33A), C33(H33C,H33D)
5.b Aromatic/amide H refined with riding coordinates:
 C23(H23), C7(H7), C29(H29), C10(H10), C2(H2), C25(H25), C3(H3), C9(H9),
 C28(H28), C21(H21), C26(H26), C18(H18), C19(H19), C20(H20), C5(H5), 
C4(H4),C13(H13), C12(H12)
5.c Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C15(H15A,H15B,H15C), 
C16(H16A,H16B,H16C), C34A(H34A,H34B,H34C), C34(H34D,H34E,H34F)
5.d Idealised tetrahedral OH refined as rotating group:
 O5(H5A), O5A(H5AA)
;