Supramolecular assemblies of new pseudohalide end-to-end bridged copper(II) complex and molecular structural variety of penta and hexa-coordinted metal(II) complexes with hydrazido-based ligand
Singh, Yogendra; Patel, R.N.; Patel, S.K.; Jadeja, R.N.; Patel, A.K.; Patel, N.; Roy, H.; Bhagriya, P.; Singh, Rita; Butcher, R.J.; Jasinski, Jerry P.; Herrero, S.; Cortijo, M.; Inorganica Chimica Acta 503 (2020) 119371–; doi:10.1016/j.ica.2019.119371

data_1565301
_publ_section_title
;
 Supramolecular assemblies of new pseudohalide end-to-end bridged
 copper(II) complex and molecular structural variety of penta and
 hexa-coordinted metal(II) complexes with hydrazido-based ligand
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119371
_journal_paper_doi               10.1016/j.ica.2019.119371
_journal_volume                  503
_journal_year                    2020
_chemical_formula_moiety         'C14 H17 Cu N4 O6, N O3'
_chemical_formula_sum            'C14 H17 Cu N5 O9'
_chemical_formula_weight         462.86
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 108.275(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.9488(7)
_cell_length_b                   11.8141(9)
_cell_length_c                   10.2189(9)
_cell_measurement_reflns_used    1743
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      71.2700
_cell_measurement_theta_min      3.7200
_cell_volume                     911.23(14)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Shelxt (Sheldrick, 2015)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 16.0416
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1055
_diffrn_reflns_av_unetI/netI     0.0481
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            2554
_diffrn_reflns_point_group_measured_fraction_full 0.742
_diffrn_reflns_point_group_measured_fraction_max 0.717
_diffrn_reflns_theta_full        67.500
_diffrn_reflns_theta_max         71.489
_diffrn_reflns_theta_min         4.557
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    2.270
_exptl_absorpt_correction_T_max  0.700
_exptl_absorpt_correction_T_min  0.355
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_exptl_crystal_colour            'pale green'
_exptl_crystal_density_diffrn    1.687
_exptl_crystal_description       chunk
_exptl_crystal_F_000             474
_exptl_crystal_size_max          0.773
_exptl_crystal_size_mid          0.459
_exptl_crystal_size_min          0.177
_refine_diff_density_max         0.722
_refine_diff_density_min         -0.493
_refine_diff_density_rms         0.100
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.00(5)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     275
_refine_ls_number_reflns         2554
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0483
_refine_ls_R_factor_gt           0.0473
_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^)+(0.0891P)^2^+0.1375P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1259
_refine_ls_wR_factor_ref         0.1277
_reflns_Friedel_coverage         0.403
_reflns_Friedel_fraction_full    0.463
_reflns_Friedel_fraction_max     0.434
_reflns_number_gt                2487
_reflns_number_total             2554
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            YS101Comp.2.cif
_cod_data_source_block           shelx
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               1565301
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              6555
_shelx_hkl_checksum              54355