Inorganic Crystal Engineering through Cation Metathesis: One-, Two-, and Three-Dimensional Cluster-Based Coordination Polymers
Zhou, Huajun; Strates, Konstantia C.; Muñoz, Miguel Á.; Little, Kevin J.; Pajerowski, Daniel M.; Meisel, Mark W.; Talham, Daniel R.; Lachgar, Abdessadek; Chemistry of Materials 19 (2007) 2238–; doi:10.1021/cm063005p

data_4001335
_publ_section_title
;
 Inorganic Crystal Engineering through Cation Metathesis:&#x00A0; One-,
 Two-, and Three-Dimensional Cluster-Based Coordination Polymers
;
_journal_issue                   9
_journal_name_full               'Chemistry of Materials'
_journal_page_first              2238
_journal_paper_doi               10.1021/cm063005p
_journal_volume                  19
_journal_year                    2007
_chemical_formula_sum            'C52 H68 Cl12 Mn2 N12 Nb6 O6'
_chemical_formula_weight         2049.92
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.1663(17)
_cell_length_b                   23.426(3)
_cell_length_c                   23.615(3)
_cell_measurement_reflns_used    1741
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      36.639
_cell_measurement_theta_min      7.732
_cell_volume                     7283.7(16)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.1494
_diffrn_reflns_av_sigmaI/netI    0.0922
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            59878
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         3.86
_exptl_absorpt_coefficient_mu    1.737
_exptl_absorpt_correction_T_max  0.9530
_exptl_absorpt_correction_T_min  0.8482
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Data were corrected for absorption effect using
multi-scan technique (SADABS). The ratio of minimum 
to maximum apparent transmission: 0.760009 
;
_exptl_crystal_colour            dark-brown
_exptl_crystal_density_diffrn    1.869
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             4048
_exptl_crystal_size_max          0.098
_exptl_crystal_size_mid          0.096
_exptl_crystal_size_min          0.028
_refine_diff_density_max         0.803
_refine_diff_density_min         -0.840
_refine_diff_density_rms         0.149
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     405
_refine_ls_number_reflns         7926
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.1014
_refine_ls_R_factor_gt           0.0620
_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^)+(0.0436P)^2^+1.6087P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1082
_refine_ls_wR_factor_ref         0.1219
_reflns_number_gt                5530
_reflns_number_total             7926
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cm063005psi20070221_113607.cif
_cod_data_source_block           a96d
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        7283.8(16)
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               4001335