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_7053179
_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 H14 K2 O19 Zr, 2(C3 H10 N3), H2 O'
_chemical_formula_sum            'C30 H36 K2 N6 O20 Zr'
_chemical_formula_weight         970.04
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.3719(7)
_cell_length_b                   21.7887(15)
_cell_length_c                   17.3292(12)
_cell_measurement_reflns_used    9799
_cell_measurement_temperature    180
_cell_measurement_theta_max      41
_cell_measurement_theta_min      3
_cell_volume                     3916.2(5)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'CrysAlis, (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    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      180
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.986
_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       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            104779
_diffrn_reflns_theta_full        40.573
_diffrn_reflns_theta_max         41.827
_diffrn_reflns_theta_min         1.869
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.583
_exptl_absorpt_correction_T_max  0.92
_exptl_absorpt_correction_T_min  0.83
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.642
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1968
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_refine_diff_density_max         3.21
_refine_diff_density_min         -0.89
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0525
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         8920
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0732
_refine_ls_R_factor_gt           0.0478
_refine_ls_shift/su_max          0.0033819
_refine_ls_shift/su_mean         0.0000865
_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: 
 1.18 1.14 0.779 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0723
_refine_ls_wR_factor_gt          0.0544
_refine_ls_wR_factor_ref         0.0530
_reflns_limit_h_max              19
_reflns_limit_h_min              0
_reflns_limit_k_max              40
_reflns_limit_k_min              0
_reflns_limit_l_max              32
_reflns_limit_l_min              0
_reflns_number_gt                9537
_reflns_number_total             13384
_reflns_threshold_expression     I>2.0\s(I)
_oxford_refine_ls_r_factor_ref   0.0449
_oxford_reflns_number_all        13373
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            c3nj00520h.txt
_cod_data_source_block           cpd7
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Other' changed to 'other'
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 b c n '
_cod_database_code               7053179
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
RIDE C   (   3,X'S) H   (  31,X'S) 
RIDE C   (   6,X'S) H   (  61,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) H   ( 142,X'S) H   ( 143,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) H   ( 153,X'S) H   ( 152,X'S) 
RIDE N   (   1,X'S) H   (  12,X'S) H   (  11,X'S) 
RIDE N   (   2,X'S) H   (  22,X'S) H   (  21,X'S) 
RIDE O   (   9,X'S) H   (  92,X'S) 
RIDE O   (  10,X'S) H   (  102,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;