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_4502074
_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         'C8 O16 Zr, 3(C7 H7 N2), K, 3(H2 O) '
_chemical_formula_sum            'C29 H27 K N6 O19 Zr'
_chemical_formula_weight         893.88
_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                100.611(13)
_cell_angle_beta                 97.694(14)
_cell_angle_gamma                93.619(13)
_cell_formula_units_Z            2
_cell_length_a                   7.1593(8)
_cell_length_b                   14.8091(16)
_cell_length_c                   16.6908(19)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    180
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2
_cell_volume                     1716.7(3)
_computing_cell_refinement       'IPDS (Stoe & Cie, 1996)'
_computing_data_collection       'IPDS (Stoe & Cie, 1996)'
_computing_data_reduction        'XRED (Stoe & Cie 1996)'
_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 0.939
_diffrn_measured_fraction_theta_max 0.930
_diffrn_measurement_device       'Stoe IPDS'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       '\f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.066
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            17029
_diffrn_reflns_theta_full        25.032
_diffrn_reflns_theta_max         26.075
_diffrn_reflns_theta_min         2.058
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.537
_exptl_absorpt_correction_T_max  0.90
_exptl_absorpt_correction_T_min  0.88
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.729
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             908
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.69
_refine_diff_density_min         -1.01
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0766
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         5136
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0538
_refine_ls_R_factor_gt           0.0408
_refine_ls_shift/su_max          0.000340
_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: 
 1.33 0.668E-01 0.721 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0528
_refine_ls_wR_factor_gt          0.0454
_refine_ls_wR_factor_ref         0.0464
_reflns_limit_h_max              8
_reflns_limit_h_min              -8
_reflns_limit_k_max              17
_reflns_limit_k_min              -18
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                4909
_reflns_number_total             6321
_reflns_threshold_expression     I>2.0\s(I)
_oxford_refine_ls_r_factor_ref   0.0425
_oxford_reflns_number_all        6300
_oxford_reflns_threshold_expression_ref I>1.5\s(I)
_cod_data_source_file            cg1009785_si_003.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_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C29 H27 K1 N6 O19 Zr1'
_cod_database_code               4502074