Self-Assembly of Zr(C2O4)44‒Metallotectons and Bisimidazolium Cations: Influence of the Dication on H-Bonded Framework Dimensionality and Material Potential Porosity
Mouchaham, Georges; Roques, Nans; Brandès, Stéphane; Duhayon, Carine; Sutter, Jean-Pascal; Crystal Growth & Design 11 (2011) 5424–; doi:10.1021/cg201008v

data_4501291
_publ_section_title
;
 Self-Assembly of Zr(C2O4)44--Metallotectons and Bisimidazolium Cations:
 Influence of the Dication on H-Bonded Framework Dimensionality and
 Material Potential Porosity
;
_journal_issue                   12
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              5424
_journal_paper_doi               10.1021/cg201008v
_journal_volume                  11
_journal_year                    2011
_chemical_formula_moiety         '2(C12 H12 N4), C8 O16 Zr, 3(H2 O)'
_chemical_formula_sum            'C32 H30 N8 O19 Zr'
_chemical_formula_weight         921.85
_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
_cell_angle_alpha                90
_cell_angle_beta                 104.3110(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.8592(4)
_cell_length_b                   13.0033(4)
_cell_length_c                   22.7481(7)
_cell_measurement_reflns_used    9833
_cell_measurement_temperature    300
_cell_measurement_theta_max      35
_cell_measurement_theta_min      2
_cell_volume                     3972.3(2)
_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      300
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.935
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_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  0.036
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            67214
_diffrn_reflns_theta_full        33.391
_diffrn_reflns_theta_max         36.295
_diffrn_reflns_theta_min         1.818
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.365
_exptl_absorpt_correction_T_max  0.95
_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    1.531
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1856
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.150
_refine_diff_density_max         1.06
_refine_diff_density_min         -0.37
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9823
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     568
_refine_ls_number_reflns         8883
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1139
_refine_ls_R_factor_gt           0.0569
_refine_ls_shift/su_max          0.0014628
_refine_ls_shift/su_mean         0.0000274
_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: 
 1.42 1.36 0.941 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1026
_refine_ls_wR_factor_gt          0.0600
_refine_ls_wR_factor_ref         0.0569
_reflns_limit_h_max              22
_reflns_limit_h_min              -22
_reflns_limit_k_max              20
_reflns_limit_k_min              0
_reflns_limit_l_max              37
_reflns_limit_l_min              0
_reflns_number_gt                10042
_reflns_number_total             17978
_reflns_threshold_expression     I>2.0\s(I)
_oxford_refine_ls_r_factor_ref   0.0518
_oxford_reflns_number_all        17949
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            cg201008v_si_007.cif
_cod_data_source_block           1
_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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_original_formula_sum        'C32 H30 N8 O19 Zr1'
_cod_database_code               4501291