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_7053175
_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         'C8 O16 Zr, 4(C3 H10 N3, 0.5(H2 O)'
_chemical_formula_sum            'C20 H41 N12 O16.5 Zr'
_chemical_formula_weight         804.84
_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   difmap
_atom_sites_solution_primary     direct
_cell_angle_alpha                84.1990(13)
_cell_angle_beta                 75.9687(18)
_cell_angle_gamma                60.221(2)
_cell_formula_units_Z            2
_cell_length_a                   10.6469(3)
_cell_length_b                   10.67004(17)
_cell_length_c                   17.8637(3)
_cell_measurement_reflns_used    36030
_cell_measurement_temperature    100
_cell_measurement_theta_max      32
_cell_measurement_theta_min      3
_cell_volume                     1708.38(7)
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_collection       'Gemini, (Oxford Diffraction, 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    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.945
_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  0.046
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            100497
_diffrn_reflns_theta_full        28.810
_diffrn_reflns_theta_max         32.371
_diffrn_reflns_theta_min         2.876
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.409
_exptl_absorpt_correction_T_max  0.92
_exptl_absorpt_correction_T_min  0.78
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.563
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         6.94
_refine_diff_density_min         -2.34
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9494
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     434
_refine_ls_number_reflns         10551
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1183
_refine_ls_R_factor_gt           0.1146
_refine_ls_shift/su_max          0.0020139
_refine_ls_shift/su_mean         0.0000260
_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: 
 27.5 10.5 14.9 11.6 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1190
_refine_ls_wR_factor_gt          0.1164
_refine_ls_wR_factor_ref         0.1159
_reflns_limit_h_max              15
_reflns_limit_h_min              -15
_reflns_limit_k_max              15
_reflns_limit_k_min              -15
_reflns_limit_l_max              26
_reflns_limit_l_min              0
_reflns_number_gt                10799
_reflns_number_total             11535
_reflns_threshold_expression     I>2.0\s(I)
_oxford_refine_ls_r_factor_ref   0.1134
_oxford_refine_ls_scale          5.185(15)
_oxford_reflns_number_all        11511
_oxford_reflns_threshold_expression_ref I>0.0\s(I)
_cod_data_source_file            c3nj00520h.txt
_cod_data_source_block           1_cpd3
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C20 H41 N12 O16.50 Zr1'
_cod_database_code               7053175
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
SUMFIX ELEMENT SCALES 
RIDE C(10,X'S) C(120,X'S) C(11,X'S) C(130,X'S) 
RIDE C(15,X'S) C(17,X'S) 
RIDE C(16,X'S) C(18,X'S) 
RIDE C(20,X'S) C(22,X'S) C(21,X'S) C(23,X'S) 
RIDE C(25,X'S) C(27,X'S) 
RIDE C(26,X'S) C(28,X'S) 
RIDE N(6,X'S) N(7,X'S) 
RIDE N(14,X'S) N(15,X'S) 
REM 
RIDE C(10,U'S) C(120,U'S) C(11,U'S) C(130,U'S) 
RIDE C(15,U'S) C(17,U'S) 
RIDE C(16,U'S) C(18,U'S) 
RIDE C(20,U'S) C(22,U'S) C(21,U'S) C(23,U'S) 
RIDE C(25,U'S) C(27,U'S) 
RIDE C(26,U'S) C(28,U'S) 
RIDE N(6,U'S) N(7,U'S) 
RIDE N(14,U'S) N(15,U'S) 
RIDE N   (   1,X'S) H   (  11,X'S) H   (  12,X'S) 
RIDE N   (   2,X'S) H   (  21,X'S) H   (  22,X'S) 
RIDE N   (   4,X'S) H   (  41,X'S) H   (  42,X'S) H   (  43,X'S) H   (  44,X'S) 
RIDE N   (   5,X'S) H   (  51,X'S) H   (  52,X'S) H   (  53,X'S) H   (  54,X'S) 
RIDE N   (   8,X'S) H   (  81,X'S) H   (  82,X'S) H   (  83,X'S) H   (  84,X'S) 
RIDE N   (   9,X'S) H   (  91,X'S) H   (  92,X'S) H   (  93,X'S) H   (  94,X'S) 
RIDE N   (  12,X'S) H   ( 121,X'S) H   ( 122,X'S) H   ( 123,X'S) H   ( 124,X'S) 
RIDE N   (  13,X'S) H   ( 131,X'S) H   ( 132,X'S) H   ( 133,X'S) H   ( 134,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                                                                             
;