Synthesis and crystal structure of bis{((E)-((4-((E)-1-(benzyloxyimino)ethyl)phenyl)imino)methyl)-2-phenolato-κ2 N,O}copper(II), C44H38CuN4O4
Huang, Jing; Ma, Jin-Xia; Wei, Ping; Zhao, Ji-Xing; Zeitschrift für Kristallographie - New Crystal Structures 234 (2019) 635–637; doi:10.1515/ncrs-2018-0589

data_8105804
_publ_section_title
;
 Synthesis and crystal structure of
 bis{((E)-((4-((E)-1-(benzyloxyimino)ethyl)phenyl)imino)methyl)-2-phenolato-\k2
 N,O}copper(II), C44H38CuN4O4
;
_journal_issue                   4
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              635
_journal_page_last               637
_journal_paper_doi               10.1515/ncrs-2018-0589
_journal_volume                  234
_journal_year                    2019
_chemical_formula_moiety         'C44 H38 Cu N4 O4'
_chemical_formula_sum            'C44 H38 Cu N4 O4'
_chemical_formula_weight         750.32
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 94.749(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.0172(13)
_cell_length_b                   10.9003(17)
_cell_length_c                   42.154(8)
_cell_measurement_reflns_used    7294
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.06
_cell_measurement_theta_min      2.37
_cell_volume                     3671.2(11)
_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    'ShelXS-1997 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0627
_diffrn_reflns_av_unetI/netI     0.0574
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            26381
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.008
_diffrn_reflns_theta_max         25.008
_diffrn_reflns_theta_min         2.105
_exptl_absorpt_coefficient_mu    0.645
_exptl_crystal_density_diffrn    1.358
_exptl_crystal_description       block
_exptl_crystal_F_000             1564
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.282
_refine_diff_density_min         -0.432
_refine_diff_density_rms         0.057
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     480
_refine_ls_number_reflns         6462
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0748
_refine_ls_R_factor_gt           0.0483
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0344P)^2^+2.6614P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0983
_refine_ls_wR_factor_ref         0.1072
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4875
_reflns_number_total             6462
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2018-0589_suppl.cif
_cod_data_source_block           20181016zh_lz3_0m_a
_cod_database_code               8105804
_shelx_estimated_absorpt_t_max   0.909
_shelx_estimated_absorpt_t_min   0.887
_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:
 C16(H16A,H16B), C38(H38A,H38B)
2.b Aromatic/amide H refined with riding coordinates:
 C22(H22), C21(H21), C20(H20), C19(H19), C18(H18), C10(H10), C9(H9), C13(H13),
 C12(H12), C7(H7), C5(H5), C4(H4), C3(H3), C2(H2), C24(H24), C25(H25), C26(H26),
  C27(H27), C29(H29), C31(H31), C32(H32), C34(H34), C35(H35), C44(H44),
 C43(H43), C42(H42), C41(H41), C40(H40)
2.c Idealised Me refined as rotating group:
 C37(H37A,H37B,H37C), C15(H15A,H15B,H15C)
;
_shelx_res_checksum              61606
_shelx_hkl_checksum              30903
_olex2_submission_special_instructions 'No special instructions were received'