Two novel copper(II) salamo-based complexes: Syntheses, X-ray crystal structures, spectroscopic properties and Hirshfeld surfaces analyses
Yu, Meng; Zhang, Yu; Pan, Ying-Qi; Wang, Li; Inorganica Chimica Acta 509 (2020) 119701–; doi:10.1016/j.ica.2020.119701

data_1564468
_publ_section_title
;
 Two novel copper(II) salamo-based complexes: Syntheses, X-ray crystal
 structures, spectroscopic properties and Hirshfeld surfaces analyses
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119701
_journal_paper_doi               10.1016/j.ica.2020.119701
_journal_volume                  509
_journal_year                    2020
_chemical_formula_moiety         'C16 H12 Cu N4 O8, C H4 O'
_chemical_formula_sum            'C17 H16 Cu N4 O9'
_chemical_formula_weight         483.87
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                90
_cell_angle_beta                 107.709(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.5463(11)
_cell_length_b                   24.841(2)
_cell_length_c                   11.6264(9)
_cell_measurement_reflns_used    4883
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.88
_cell_measurement_theta_min      2.46
_cell_volume                     3726.9(5)
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0724
_diffrn_reflns_av_unetI/netI     0.0719
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            23654
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.013
_exptl_absorpt_coefficient_mu    1.236
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8956
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.725
_exptl_crystal_description       block
_exptl_crystal_F_000             1976
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.958
_refine_diff_density_min         -0.503
_refine_diff_density_rms         0.119
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     565
_refine_ls_number_reflns         6559
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.1063
_refine_ls_R_factor_gt           0.0682
_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^)+(0.0297P)^2^+16.8621P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1242
_refine_ls_wR_factor_ref         0.1401
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4759
_reflns_number_total             6559
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2020-509-119701.cif
_cod_data_source_block           22_a
_cod_depositor_comments
;

2022-05-06
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C34 H32 Cu2 N8 O18'
_cod_original_formula_weight         967.75
_cod_original_formula_moiety    'C16 H12 Cu N4 O8, C17 H16 Cu N4 O9, C H4 O'
_cod_original_formula_units_Z            4
_cod_database_code               1564468
_shelx_estimated_absorpt_t_max   0.827
_shelx_estimated_absorpt_t_min   0.781
_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, All O(H) groups
2. Restrained distances
 O17-H17
 0.87 with sigma of 0.01
 C33-H17
 1.872094 with sigma of 0.02
 Cu2-H17
 2.873486 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C24(H24A,H24B), C25(H25A,H25B)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C7(H7), C10(H10), C12(H12), C14(H14), C15(H15),
 C18(H18), C19(H19), C21(H21), C23(H23), C26(H26), C28(H28), C30(H30), C31(H31)
3.c Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C), C34(H34A,H34B,H34C)
3.d Idealised tetrahedral OH refined as rotating group:
 O18(H18A)
;
_shelx_res_checksum              71653
_shelx_hkl_checksum              81800