Extended H-bond networks based on guanidinium H-donors and [Zr(A)4]4− H-acceptor units: modulation of the assemblage and guest accessible volume by chemical design (A = oxalate, dihydrobenzoquinonate, chloranilate)
Mouchaham, Georges; Roques, Nans; Duhayon, Carine; Imaz, Inhar; Sutter, Jean-Pascal; New Journal of Chemistry 37 (2013) 3476–; doi:10.1039/c3nj00520h

data_7053174
_publ_section_title
;
 Extended H-bond networks based on guanidinium H-donors and
 [Zr(A)4]4&#x2212; H-acceptor units: modulation of the assemblage and
 guest accessible volume by chemical design (A = oxalate,
 dihydrobenzoquinonate, chloranilate)
;
_journal_issue                   11
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              3476
_journal_paper_doi               10.1039/c3nj00520h
_journal_volume                  37
_journal_year                    2013
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C8 O16 Zr, 4(C3 H6 N3), 5(H2 O)'
_chemical_formula_sum            'C20 H34 N12 O21 Zr'
_chemical_formula_weight         869.78
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   37.6265(11)
_cell_length_b                   7.2895(2)
_cell_length_c                   12.4055(4)
_cell_measurement_reflns_used    9767
_cell_measurement_temperature    180
_cell_measurement_theta_max      35
_cell_measurement_theta_min      3
_cell_volume                     3402.56(18)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.026
_diffrn_reflns_limit_h_max       60
_diffrn_reflns_limit_h_min       -60
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            59891
_diffrn_reflns_theta_full        35.061
_diffrn_reflns_theta_max         35.061
_diffrn_reflns_theta_min         1.082
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.428
_exptl_absorpt_correction_T_max  0.92
_exptl_absorpt_correction_T_min  0.88
_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    1.698
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1784
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.48
_refine_diff_density_min         -0.51
_refine_ls_abs_structure_details 'Flack (1983), 6037 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.273(15)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0823
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     488
_refine_ls_number_reflns         11443
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0376
_refine_ls_R_factor_gt           0.0296
_refine_ls_shift/su_max          0.0043019
_refine_ls_shift/su_mean         0.0001211
_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: 
 1.23 0.393 1.02 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0346
_refine_ls_wR_factor_gt          0.0316
_refine_ls_wR_factor_ref         0.0309
_reflns_limit_h_max              60
_reflns_limit_h_min              0
_reflns_limit_k_max              11
_reflns_limit_k_min              0
_reflns_limit_l_max              19
_reflns_limit_l_min              -20
_reflns_number_gt                12116
_reflns_number_total             13840
_reflns_threshold_expression     I>2.0\s(I)
_oxford_refine_ls_r_factor_ref   0.0269
_oxford_reflns_number_all        13811
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            c3nj00520h.txt
_cod_data_source_block           cpd2
_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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        3402.56(17)
_cod_original_sg_symbol_H-M      'P n a 21 '
_cod_original_formula_sum        'C20 H34 N12 O21 Zr1'
_cod_database_code               7053174