Di-μ-azido-diazidodi-μ-oxalato-dihistaminetetracopper(II) 0.9-hydrate
Liu, Chen; Abboud, Khalil A.; Acta Crystallographica Section E 69 (2013) m337–m338; doi:10.1107/S1600536813013329

data_2237936
_publ_section_title
;
 Di-\m-azido-diazidodi-\m-oxalato-dihistaminetetracopper(II) 0.9-hydrate
;
_journal_coeditor_code           LH5597
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m337
_journal_page_last               m338
_journal_paper_doi               10.1107/S1600536813013329
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          '[Cu4 (C2 O4)2 (N3)4 (C5 H9 N3)2], 0.9H2 O'
_chemical_formula_moiety         'C14 H18 Cu4 N18 O8, 0.9(H2 O)'
_chemical_formula_sum            'C14 H19.8 Cu4 N18 O8.9'
_chemical_formula_weight         838.62
_chemical_name_systematic
;
Di-\m-azido-diazidodi-\m-oxalato-dihistaminetetracopper(II) 0.9-hydrate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                106.005(2)
_cell_angle_beta                 91.715(2)
_cell_angle_gamma                115.010(2)
_cell_formula_units_Z            1
_cell_length_a                   7.7003(10)
_cell_length_b                   8.2841(11)
_cell_length_c                   11.8677(15)
_cell_measurement_reflns_used    29
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.0
_cell_measurement_theta_min      2.0
_cell_volume                     650.07(15)
_computing_cell_refinement       'SAINT (Bruker, 2008)'
_computing_data_collection       'APEX2 (Bruker, 2008)'
_computing_data_reduction        'SAINT (Bruker, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0414
_diffrn_reflns_av_sigmaI/netI    0.0409
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            5770
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.81
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.313
_exptl_absorpt_correction_T_max  0.8771
_exptl_absorpt_correction_T_min  0.6540
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
'[based on measured indexed crystal faces (SHELXTL; Sheldrick, 2008)]'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.137
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             416
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.602
_refine_diff_density_min         -0.564
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     238
_refine_ls_number_reflns         2885
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_gt           0.0287
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0327P)^2^+0.5471P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0695
_refine_ls_wR_factor_ref         0.0732
_reflns_number_gt                2442
_reflns_number_total             2885
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lh5597.cif
_cod_data_source_block           I
_cod_database_code               2237936
_cod_database_fobs_code          2237936