Synthesis and crystal structure of bis{1-(((4-(1-(hydroxyimino)ethyl)phenyl)imino)methyl)naphthalen-2-olato-κ2 O,N}copper(II), C38H30CuN4O4
Li, Peng-Peng; Zhao, Li; Zhao, Ji-Xing; Zhu, Zhao-Bin; Wang, Fei; An, Qin-Qin; Zeitschrift für Kristallographie - New Crystal Structures 232 (2017) 889–890; doi:10.1515/ncrs-2017-0044

data_8106710
_publ_section_title
;
 Synthesis and crystal structure of
 bis{1-(((4-(1-(hydroxyimino)ethyl)phenyl)imino)methyl)naphthalen-2-olato-\k2
 O,N}copper(II), C38H30CuN4O4
;
_journal_issue                   6
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              889
_journal_page_last               890
_journal_paper_doi               10.1515/ncrs-2017-0044
_journal_volume                  232
_journal_year                    2017
_chemical_formula_moiety         'C38 H30 Cu N4 O4'
_chemical_formula_sum            'C38 H30 Cu N4 O4'
_chemical_formula_weight         670.20
_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     iterative
_cell_angle_alpha                89.960(10)
_cell_angle_beta                 69.689(10)
_cell_angle_gamma                80.269(8)
_cell_formula_units_Z            1
_cell_length_a                   8.3882(7)
_cell_length_b                   8.5024(9)
_cell_length_c                   11.3649(15)
_cell_measurement_reflns_used    540
_cell_measurement_temperature    294.68(10)
_cell_measurement_theta_max      20.7150
_cell_measurement_theta_min      3.7500
_cell_volume                     747.73(15)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      294.68(10)
_diffrn_detector_area_resol_mean 16.0733
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
  1 omega   -4.00   24.50   1.5000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.3571  -99.0000  120.0000 19

  2 omega   24.00   55.50   1.5000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.3571   38.0000  -90.0000 21

  3 omega  -46.00   50.00   1.5000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7946  -77.0000 -120.0000 64

  4 omega   -7.00   89.00   1.5000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7946   77.0000    0.0000 64

  5 omega    3.00   43.50   1.5000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7946   77.0000   90.0000 27

  6 omega  -48.00   27.00   1.5000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7946  -57.0000  120.0000 50
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0256971000
_diffrn_orient_matrix_UB_12      0.0840998000
_diffrn_orient_matrix_UB_13      0.0017383000
_diffrn_orient_matrix_UB_21      0.0772628000
_diffrn_orient_matrix_UB_22      0.0108037000
_diffrn_orient_matrix_UB_23      0.0087329000
_diffrn_orient_matrix_UB_31      0.0420965000
_diffrn_orient_matrix_UB_32      -0.0017277000
_diffrn_orient_matrix_UB_33      -0.0660833000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0644
_diffrn_reflns_av_unetI/netI     0.1612
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4922
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.014
_diffrn_reflns_theta_min         3.762
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.782
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.37929
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark brown'
_exptl_crystal_density_diffrn    1.488
_exptl_crystal_description       plate
_exptl_crystal_F_000             347
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.308
_refine_diff_density_min         -0.354
_refine_diff_density_rms         0.067
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.983
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     216
_refine_ls_number_reflns         2937
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.983
_refine_ls_R_factor_all          0.1681
_refine_ls_R_factor_gt           0.0701
_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^)+(0.0197P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0943
_refine_ls_wR_factor_ref         0.1308
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1377
_reflns_number_total             2937
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2017-0044_suppl.cif
_cod_data_source_block           d529
_cod_database_code               8106710
_reflns_odcompleteness_completeness 99.44
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2A), C3(H3), C5(H5), C6(H6), C7(H7), C8(H8), C11(H11), C13(H13), C14(H14),
  C16(H16), C17(H17)
2.b Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C)
2.c Idealised tetrahedral OH refined as rotating group:
 O2(H2)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'