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_7053178
_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_formula_moiety         'C24 Cl8 O16 Zr, 4(C3 H6 N3), H2 O '
_chemical_formula_sum            'C36 H26 Cl8 N12 O17 Zr'
_chemical_formula_weight         1273.51
_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                 111.033(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.4105(4)
_cell_length_b                   20.2998(5)
_cell_length_c                   13.9896(4)
_cell_measurement_reflns_used    26113
_cell_measurement_temperature    180
_cell_measurement_theta_max      29
_cell_measurement_theta_min      3
_cell_volume                     4614.9(2)
_computing_cell_refinement       'CrysAlis RED, (Oxford Diffraction, 2002)'
_computing_data_collection       'Gemini, (Oxford Diffraction, 2006)'
_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 0.925
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction Gemini'
_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  0.053
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            81922
_diffrn_reflns_theta_full        26.859
_diffrn_reflns_theta_max         29.194
_diffrn_reflns_theta_min         3.379
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.790
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.85
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, acta cryst. (1995), a51, 33-38'
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.833
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       planar
_exptl_crystal_F_000             2552
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.40
_refine_diff_density_min         -0.32
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     667
_refine_ls_number_reflns         6799
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_gt           0.0258
_refine_ls_shift/su_max          0.0025673
_refine_ls_shift/su_mean         0.0000679
_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: 
 8.40 -5.04 6.41 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0369
_refine_ls_wR_factor_gt          0.0273
_refine_ls_wR_factor_ref         0.0255
_reflns_limit_h_max              22
_reflns_limit_h_min              -23
_reflns_limit_k_max              27
_reflns_limit_k_min              0
_reflns_limit_l_max              19
_reflns_limit_l_min              0
_reflns_number_gt                7587
_reflns_number_total             11560
_reflns_threshold_expression     I>2.0\s(I)
_oxford_refine_ls_r_factor_ref   0.0230
_oxford_reflns_number_all        11541
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            c3nj00520h.txt
_cod_data_source_block           cpd6
_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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_original_formula_sum        'C36 H26 Cl8 N12 O17 Zr1'
_cod_database_code               7053178