Hydrogen-bonded supramolecular architectures based on [Zr(C2O4)4]4− anion and protonated polyamine cations
Hamdouni, Monia; Walha, Siwar; Duhayon, Carine; Kabadou, Ahlem; Sutter, Jean-Pascal; CrystEngComm 19 (2017) 1633–; doi:10.1039/C6CE02547A

data_7227808
_publ_section_title
;
 Hydrogen-bonded supramolecular architectures based on
 [Zr(C2O4)4]4&#x2212; anion and protonated polyamine cations
;
_journal_issue                   12
_journal_name_full               CrystEngComm
_journal_page_first              1633
_journal_paper_doi               10.1039/C6CE02547A
_journal_volume                  19
_journal_year                    2017
_chemical_formula_moiety         'C8 O16 Zr, 2(C6 H10 N2), 4(H2 O)'
_chemical_formula_sum            'C20 H28 N4 O20 Zr'
_chemical_formula_weight         735.68
_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   difmap
_atom_sites_solution_primary     direct
_audit_update_record
;
2016-11-15 deposited with the CCDC.
2017-02-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.917(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.078(5)
_cell_length_b                   20.979(5)
_cell_length_c                   8.776(5)
_cell_measurement_reflns_used    9636
_cell_measurement_temperature    180
_cell_measurement_theta_max      35
_cell_measurement_theta_min      2
_cell_volume                     2742.5(19)
_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    'SHELXS 86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      180
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.975
_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  0.058
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            43277
_diffrn_reflns_theta_full        25.060
_diffrn_reflns_theta_max         35.800
_diffrn_reflns_theta_min         2.375
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.503
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.79
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            'blue violet'
_exptl_crystal_density_diffrn    1.782
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.44
_refine_diff_density_min         -0.41
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1223
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         6566
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0842
_refine_ls_R_factor_gt           0.0397
_refine_ls_shift/su_max          0.0010708
_refine_ls_shift/su_mean         0.0000930
_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: 
 0.326 0.342 0.288 0.164 0.722E-01 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0624
_refine_ls_wR_factor_gt          0.0315
_refine_ls_wR_factor_ref         0.0295
_reflns_limit_h_max              24
_reflns_limit_h_min              -24
_reflns_limit_k_max              33
_reflns_limit_k_min              0
_reflns_limit_l_max              14
_reflns_limit_l_min              0
_reflns_number_gt                7226
_reflns_number_total             12503
_reflns_threshold_expression     I>2.0\s(I)
_oxford_refine_ls_r_factor_ref   0.0352
_oxford_reflns_number_all        12486
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            c6ce02547a2.cif
_cod_data_source_block           cpd2
_cod_depositor_comments
'Adding full bibliography for 7227806--7227809.cif.'
_cod_original_cell_volume        2742.5(16)
_cod_original_sg_symbol_Hall     '-P 2ybc '
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_original_formula_sum        'C20 H28 N4 O20 Zr1'
_cod_database_code               7227808