Modular Assembling of [Zr(C2O4)4]4−and [DabcoH2]2+Units in Supramolecular Hybrid Architectures Including an Open Framework with Reversible Sorption Properties (Dabco = 1,4-Diazabicyclo[2. 2. 2]octane)
Thétiot, Franck; Duhayon, Carine; Venkatakrishnan, Thengarai S.; Sutter, Jean-Pascal; Crystal Growth & Design 8 (2008) 1870–; doi:10.1021/cg700971n

data_4503290
_publ_section_title
;
 Modular Assembling of [Zr(C2O4)4]4&#x2212;and [DabcoH2]2+Units in
 Supramolecular Hybrid Architectures Including an Open Framework with
 Reversible Sorption Properties (Dabco = 1,4-Diazabicyclo[2. 2. 2]octane)
;
_journal_issue                   6
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              1870
_journal_paper_doi               10.1021/cg700971n
_journal_volume                  8
_journal_year                    2008
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C8 K2 O16 Zr, C6 H14 N2, 6.5(H2 O)'
_chemical_formula_sum            'C14 H27 K2 N2 O22.5 Zr'
_chemical_formula_weight         752.78
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             06-07-28
_audit_creation_method           CRYSTALS_ver_12.51
_cell_angle_alpha                90
_cell_angle_beta                 99.509(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.225(5)
_cell_length_b                   19.053(5)
_cell_length_c                   13.954(5)
_cell_measurement_reflns_used    5200
_cell_measurement_temperature    180
_cell_measurement_theta_max      29
_cell_measurement_theta_min      3
_cell_volume                     2681.1(18)
_computing_cell_refinement       'CrysAlis RED, (Oxford Diffraction, 2002)'
_computing_data_collection       'Xcalibur, (Oxford Diffraction, 2002)'
_computing_data_reduction        'CrysAlis RED, (Oxford Diffraction, 2002)'
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Oxford Diffraction XCALIBUR'
_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       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            23433
_diffrn_reflns_theta_full        29.070
_diffrn_reflns_theta_max         29.070
_diffrn_reflns_theta_min         3.139
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.822
_exptl_absorpt_correction_T_max  0.85
_exptl_absorpt_correction_T_min  0.66
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.832
_exptl_crystal_description       block
_exptl_crystal_F_000             1480
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.23
_refine_diff_density_min         -0.95
_refine_ls_abs_structure_details 'Flack (1983), 2188 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.29(4)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0289
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     684
_refine_ls_number_reflns         8964
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0513
_refine_ls_R_factor_gt           0.0432
_refine_ls_shift/su_max          0.000271
_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: 
 4.80 -0.693 3.34 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0585
_refine_ls_wR_factor_gt          0.0540
_refine_ls_wR_factor_ref         0.0540
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              26
_reflns_limit_k_min              -21
_reflns_limit_l_max              19
_reflns_limit_l_min              0
_reflns_number_gt                8964
_reflns_number_total             11152
_reflns_threshold_expression     I>3.0\s(I)
_cod_data_source_file            cg700971n-file004.cif
_cod_data_source_block           Compd_1_cif
_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 1 '
_cod_original_formula_sum        'C14 H27 K2 N2 O22.50 Zr1'
_cod_database_code               4503290