Driving the Assembling of Zirconium Tetraoxalate Metallotectons and Benzimidazolium Cations: From Three Dimensional Hydrogen-Bonded Compact Architectures to Open-Frameworks
Mouchaham, Georges; Roques, Nans; Imaz, Inhar; Duhayon, Carine; Sutter, Jean-Pascal; Crystal Growth & Design 10 (2010) 4906–; doi:10.1021/cg1009785

data_4502079
_publ_section_title
;
 Driving the Assembling of Zirconium Tetraoxalate Metallotectons and
 Benzimidazolium Cations: From Three Dimensional Hydrogen-Bonded Compact
 Architectures to Open-Frameworks
;
_journal_issue                   11
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              4906
_journal_paper_doi               10.1021/cg1009785
_journal_volume                  10
_journal_year                    2010
_chemical_formula_moiety         '(C14 O28 Zr2), 6(C7 H6 Cl N2), 13.5(H2 O)'
_chemical_formula_sum            'C56 H63 Cl6 N12 O41.5 Zr2'
_chemical_formula_weight         1963.33
_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
_cell_angle_alpha                88.350(4)
_cell_angle_beta                 88.096(5)
_cell_angle_gamma                86.067(5)
_cell_formula_units_Z            2
_cell_length_a                   13.3247(14)
_cell_length_b                   15.3217(16)
_cell_length_c                   19.237(2)
_cell_measurement_reflns_used    9901
_cell_measurement_temperature    180
_cell_measurement_theta_max      28
_cell_measurement_theta_min      3
_cell_volume                     3914.6(7)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      180
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device       'Bruker Kappa Apex2'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.042
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            57089
_diffrn_reflns_theta_full        27.045
_diffrn_reflns_theta_max         27.597
_diffrn_reflns_theta_min         1.059
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.576
_exptl_absorpt_correction_T_max  0.94
_exptl_absorpt_correction_T_min  0.89
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, acta cryst. (1995), a51, 33-38'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.666
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       planar
_exptl_crystal_F_000             1970
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.12
_refine_diff_density_min         -0.77
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1113
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1079
_refine_ls_number_reflns         11101
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0873
_refine_ls_R_factor_gt           0.0530
_refine_ls_shift/su_max          0.001343
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 0.799 0.573 0.470 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0802
_refine_ls_wR_factor_gt          0.0531
_refine_ls_wR_factor_ref         0.0506
_reflns_limit_h_max              17
_reflns_limit_h_min              -17
_reflns_limit_k_max              19
_reflns_limit_k_min              -19
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                12199
_reflns_number_total             17504
_reflns_threshold_expression     I>2.0\s(I)
_oxford_refine_ls_r_factor_ref   0.0479
_oxford_reflns_number_all        17449
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            cg1009785_si_008.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        3914.7(7)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C56 H63 Cl6 N12 O41.50 Zr2'
_cod_database_code               4502079