Synthesis and crystal structure of bis{2-bromo-6-((E)-((4-((E)-1-(methoxy-imino)ethyl)phenyl)imino)methyl)phenolato- κ 2 N,O}zinc(II)-methanol(1/2), C65H60Br4N8O9Zn2
Song, Xiao-San; Zeitschrift für Kristallographie - New Crystal Structures 236 (2021) 93–95; doi:10.1515/ncrs-2020-0370

data_8104891
_publ_section_title
;
 Synthesis and crystal structure of
 bis{2-bromo-6-((E)-((4-((E)-1-(methoxy-imino)ethyl)phenyl)imino)methyl)phenolato-
 \k 2 N,O}zinc(II)-methanol(1/2), C65H60Br4N8O9Zn2
;
_journal_issue                   1
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              93
_journal_page_last               95
_journal_paper_doi               10.1515/ncrs-2020-0370
_journal_volume                  236
_journal_year                    2021
_chemical_formula_moiety         '2(C32 H28 Br2 N4 O4 Zn), C H4 O'
_chemical_formula_sum            'C65 H60 Br4 N8 O9 Zn2'
_chemical_formula_weight         1547.59
_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   mixed
_atom_sites_solution_primary     dual
_cell_angle_alpha                92.654(2)
_cell_angle_beta                 104.4460(10)
_cell_angle_gamma                116.0400(10)
_cell_formula_units_Z            1
_cell_length_a                   10.5707(4)
_cell_length_b                   11.1159(5)
_cell_length_c                   15.9260(7)
_cell_measurement_reflns_used    8195
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.89
_cell_measurement_theta_min      2.45
_cell_volume                     1601.90(12)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0360
_diffrn_reflns_av_unetI/netI     0.0435
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            17933
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.021
_diffrn_reflns_theta_min         2.245
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.306
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.5488
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_density_diffrn    1.604
_exptl_crystal_description       block
_exptl_crystal_F_000             778
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.892
_refine_diff_density_min         -0.597
_refine_diff_density_rms         0.087
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     447
_refine_ls_number_reflns         6290
_refine_ls_number_restraints     99
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0836
_refine_ls_R_factor_gt           0.0574
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0339P)^2^+4.7750P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1150
_refine_ls_wR_factor_ref         0.1284
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4763
_reflns_number_total             6290
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2020-0370_suppl.cif
_cod_data_source_block           1
_cod_database_code               8104891
_shelx_estimated_absorpt_t_max   0.692
_shelx_estimated_absorpt_t_min   0.655
_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, All O(H,H) groups
2. Restrained distances
 C33A-O5
 1.45 with sigma of 0.01
 O2-C16 \\sim O2A-C16A
 with sigma of 0.02
 C33A-O5 \\sim O5-C33
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O2A \\sim O4A \\sim N2A \\sim C32A \\sim C33 \\sim C33A: within 3.8A with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C33A) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(O4A)
\\sim Ueq, Uanis(C32A) \\sim Ueq, Uanis(N4A) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(N2) = Uanis(N2A)
Uanis(O2A) = Uanis(O2)
Uanis(N4) = Uanis(N4A)
Uanis(O4) = Uanis(O4A)
Uanis(C32) = Uanis(C32A)
4. Rigid body (RIGU) restrains
 O2, O4, N2, N4, C16, C32, C33
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O2A, O4A, N2A, N4A, C16A, C32A, C33A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(O2A)=Sof(N2A)=Sof(C16A)=Sof(H16D)=Sof(H16E)=Sof(H16F)=1-FVAR(1)
 Sof(O2)=Sof(N2)=Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(H16C)=FVAR(1)
 Sof(O4A)=Sof(N4A)=Sof(C32A)=Sof(H32D)=Sof(H32E)=Sof(H32F)=1-FVAR(2)
 Sof(O4)=Sof(N4)=Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(H32C)=FVAR(2)
 Fixed Sof: O5(0.5) H5A(0.25) H5B(0.25) C33(0.25) H33B(0.25) H33A(0.25)
 H33C(0.25) C33A(0.25) H33D(0.25) H33E(0.25) H33F(0.25)
6.a Riding coordinates:
 C33(H33B,H33A,H33C), C33A(H33D,H33E,H33F)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C7(H7), C9(H9), C10(H10), C12(H12), C13(H13),
 C19(H19), C20(H20), C21(H21), C23(H23), C25(H25), C26(H26), C28(H28), C29(H29)
6.c Tetrahedral OH refined with riding coordinates:
 O5(H5A), O5(H5B)
6.d Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C16A(H16D,H16E,H16F), C31(H31A,H31B,
 H31C), C32(H32A,H32B,H32C), C32A(H32D,H32E,H32F)
;