Solvent controlled nuclearity in Cu(ii) complexes linked by the CO32− ligand: synthesis, structure and magnetic properties
Rodríguez, Montserrat; Llobet, Antoni; Corbella, Montserrat; Müller, Peter; Usón, Miguel Angel; Martell, Arthur E.; Reibenspies, Joseph; Journal of the Chemical Society, Dalton Transactions  (2002) 2900–; doi:10.1039/b203057h

data_7011697
_publ_section_title
;
 Solvent controlled nuclearity in Cu(ii) complexes linked by the
 CO32&#x2212; ligand: synthesis, structure and magnetic properties
;
_journal_issue                   14
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2900
_journal_paper_doi               10.1039/b203057h
_journal_year                    2002
_chemical_formula_moiety
'[Cu4(m4-CO3)(m-Cl)2(ClO4)2(dpt)4(OH2)](ClO4)2.3CH3OH'
_chemical_formula_sum            'C28 H80 Cl6 Cu4 N12 O22'
_chemical_formula_weight         1403.90
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.02(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.798(3)
_cell_length_b                   17.105(3)
_cell_length_c                   25.802(5)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    133(2)
_cell_volume                     5617(2)
_computing_cell_refinement       'Siemens SAINT (V. 5.00, Siemens 1998)'
_computing_data_collection       'Siemens SMART (V. 4.202, Siemens 1996)'
_computing_data_reduction        'Siemens SAINT (V. 5.00, Siemens 1998)'
_computing_molecular_graphics    'SHELXTL-Plus (Bruker)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_detector_area_resol_mean '8192 pixels/mm'
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type
'Stoe Siemens-Huber four circle diffractometer'
_diffrn_measurement_method       'phi and omega scan'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0359
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9571
_diffrn_reflns_theta_full        24.71
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         1.98
_exptl_absorpt_coefficient_mu    1.859
_exptl_absorpt_correction_type   'multi-scan, semiempirical (SADABS)'
_exptl_crystal_colour            'deep blue'
_exptl_crystal_density_diffrn    1.660
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2904
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.5
_refine_diff_density_max         0.939
_refine_diff_density_min         -0.489
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     737
_refine_ls_number_reflns         9571
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.145
_refine_ls_R_factor_all          0.0662
_refine_ls_R_factor_gt           0.0472
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0281P)^2^+15.0174P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0918
_refine_ls_wR_factor_ref         0.0991
_reflns_number_gt                7740
_reflns_number_total             9571
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b203057h.txt
_cod_data_source_block           m-te
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0281P)^2^+15.0174P] 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^)+(0.0281P)^2^+15.0174P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7011697