Product of a DMF Aminalization, Bis[bis(3,5-dimethylpyrazol-1-yl)(dimethylamino)methane]copper(II) Perchlorate-Bis(dichloromethane)
Robert T. Stibrany; Spencer Knapp; Joseph A. Potenza; Harvey J. Schugar; Inorganic Chemistry 38 (1999) 132–135; doi:10.1021/ic980903h

data_4321722
_publ_section_title
;
 Product of a DMF Aminalization,
 Bis[bis(3,5-dimethylpyrazol-1-yl)(dimethylamino)methane]copper(II)
 Perchlorate-Bis(dichloromethane)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              132
_journal_page_last               135
_journal_paper_doi               10.1021/ic980903h
_journal_volume                  38
_journal_year                    1999
_chemical_compound_source        synthesized
_chemical_formula_sum            'C28 H46 Cl6 Cu N10 O8'
_chemical_formula_weight         926.99
_chemical_name_systematic
;
 Bis([bis(3,5-dimethylpyrazol-1-yl)
 (dimethylamino)methane]copper(II)perchlorate Bis(dichloromethane)
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   'geom and difference Fourier '
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 120.73(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   26.278(5)
_cell_length_b                   8.835(2)
_cell_length_c                   20.655(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_volume                     4122.0(19)
_computing_cell_refinement       'Enraf-Nonius SDP (1983)'
_computing_data_collection       'Enraf-Nonius SDP (1983)'
_computing_data_reduction        'Enraf-Nonius SDP (1983)'
_computing_molecular_graphics    'ORTEPII. (Johnson, 1976)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf-Nonius CAD4 diffractometer '
_diffrn_measurement_method       'theta-two theta '
_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  0.0137
_diffrn_reflns_av_sigmaI/netI    0.0301
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            2593
_diffrn_reflns_theta_max         21.97
_diffrn_reflns_theta_min         2.07
_diffrn_standards_decay_%        +/-0.4%
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.976
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.899
_exptl_absorpt_correction_type   'empirical, psi scan '
_exptl_crystal_colour            'pale green '
_exptl_crystal_density_diffrn    1.494
_exptl_crystal_description       block
_exptl_crystal_F_000             1916
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.553
_refine_diff_density_min         -0.426
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.038
_refine_ls_goodness_of_fit_obs   1.062
_refine_ls_hydrogen_treatment    'H coordinates refined '
_refine_ls_matrix_type           full
_refine_ls_number_parameters     297
_refine_ls_number_reflns         2527
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.050
_refine_ls_restrained_S_obs      1.077
_refine_ls_R_factor_all          0.0716
_refine_ls_R_factor_obs          0.0492
_refine_ls_shift/esd_max         3.138
_refine_ls_shift/esd_mean        0.223
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0640P)^2^+18.2556P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1371
_refine_ls_wR_factor_obs         0.1221
_reflns_number_observed          1979
_reflns_number_total             2527
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic980903h.cif
_cod_data_source_block           pyy6IC980903H
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0640P)^2^+18.2556P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0640P)^2^+18.2556P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        4121.9(14)
_cod_database_code               4321722