Synthesis and structures of carboxylate-bridged polynuclear copper(II)‒lanthanide(III) complexes [CuLn(C5H5N+CH2CO2−)5(H2O)5][ClO4]5·2H2O (Ln = La or Nd) and [Cu3Nd2(C5H5N+CH2CO2−)10(NO3)2(H2O)8][ClO4]10·4H2O
Yang, Yang-Yi; Wu, Yu-Luan; Long, La-Sheng; Chen, Xiao-Ming; Journal of the Chemical Society, Dalton Transactions  (1999) 2005–; doi:10.1039/a900647h

data_7027281
_publ_section_title
;
 Synthesis and structures of carboxylate-bridged polynuclear
 copper(II)--lanthanide(III) complexes
 [CuLn(C5H5N+CH2CO2&#x2212;)5(H2O)5][ClO4]5&#x00B7;2H2O
 (Ln&#x2005;=&#x2005;La or Nd) and
 [Cu3Nd2(C5H5N+CH2CO2&#x2212;)10(NO3)2(H2O)8][ClO4]10&#x00B7;4H2O
;
_journal_issue                   12
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2005
_journal_paper_doi               10.1039/a900647h
_journal_year                    1999
_chemical_formula_sum            'C70 H94 Cl10 Cu3 N12 Nd2 O78'
_chemical_formula_weight         3185.17
_chemical_name_systematic
; 
 ? 
;
_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                73.380(10)
_cell_angle_beta                 72.140(10)
_cell_angle_gamma                88.900(10)
_cell_formula_units_Z            1
_cell_length_a                   11.410(4)
_cell_length_b                   14.992(6)
_cell_length_c                   18.447(7)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      7.5
_cell_volume                     2869.8(19)
_computing_cell_refinement       'SHELXTL-Plus (Sheldrick, 1990)'
_computing_data_collection       'SHELXTL-Plus (Sheldrick, 1990)'
_computing_data_reduction        'SHELXTL-Plus (Sheldrick, 1990)'
_computing_molecular_graphics    'Ortep3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Siemens R3'
_diffrn_measurement_method       '\w 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  0.0127
_diffrn_reflns_av_sigmaI/netI    0.0525
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            11282
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.12
_diffrn_standards_decay_%        1.5
_diffrn_standards_interval_count 120
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.789
_exptl_absorpt_correction_T_max  0.6158
_exptl_absorpt_correction_T_min  0.4682
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'deep blue'
_exptl_crystal_density_diffrn    1.843
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       polyhedral
_exptl_crystal_F_000             1599
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.170
_refine_diff_density_min         -1.270
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     826
_refine_ls_number_reflns         11263
_refine_ls_number_restraints     95
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0733
_refine_ls_R_factor_gt           0.0502
_refine_ls_shift/su_max          2.738
_refine_ls_shift/su_mean         0.040
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0689P)^2^+4.3474P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1212
_refine_ls_wR_factor_ref         0.1344
_reflns_number_gt                8654
_reflns_number_total             11263
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            900647hsup1.cif
_cod_data_source_block           complex_2
_cod_depositor_comments
;
The following automatic conversions were performed:
'__refine_special_details' tag replaced with
'_refine_special_details'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0689P)^2^+4.3474P] 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^)+(0.0689P)^2^+4.3474P] 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      P-1
_cod_database_code               7027281