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_7227807
_publ_section_title
;
 Hydrogen-bonded supramolecular architectures based on
 [Zr(C2O4)4]4&#x2212; anion and protonated polyamine cations
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_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, 4(C5 H7 N2), 2(H2 O)'
_chemical_formula_sum            'C28 H32 N8 O18 Zr'
_chemical_formula_weight         859.82
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_update_record
;
2017-01-23 deposited with the CCDC.
2017-02-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.3052(16)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.0194(4)
_cell_length_b                   17.8877(10)
_cell_length_c                   13.4593(8)
_cell_measurement_reflns_used    9789
_cell_measurement_temperature    100
_cell_measurement_theta_max      31
_cell_measurement_theta_min      2
_cell_volume                     1689.94(17)
_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    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            53638
_diffrn_reflns_theta_full        30.520
_diffrn_reflns_theta_max         30.520
_diffrn_reflns_theta_min         2.277
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.421
_exptl_absorpt_correction_T_max  0.94
_exptl_absorpt_correction_T_min  0.90
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.690
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.48
_refine_diff_density_min         -0.34
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0630
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     249
_refine_ls_number_reflns         5077
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0200
_refine_ls_R_factor_gt           0.0198
_refine_ls_shift/su_max          0.0019536
_refine_ls_shift/su_mean         0.0000831
_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: 
 0.118 0.871E-01 0.416E-01 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0206
_refine_ls_wR_factor_gt          0.0202
_refine_ls_wR_factor_ref         0.0201
_reflns_limit_h_max              10
_reflns_limit_h_min              -10
_reflns_limit_k_max              25
_reflns_limit_k_min              0
_reflns_limit_l_max              19
_reflns_limit_l_min              0
_reflns_number_gt                5095
_reflns_number_total             5156
_reflns_threshold_expression     I>2.0\s(I)
_oxford_refine_ls_r_factor_ref   0.0197
_oxford_reflns_number_all        5141
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            c6ce02547a2.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Other' changed to 'other'
according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7227806--7227809.cif.
;
_cod_original_cell_volume        1689.94(10)
_cod_original_sg_symbol_Hall     '-P 2yac '
_cod_original_sg_symbol_H-M      'P 1 2/n 1 '
_cod_original_formula_sum        'C28 H32 N8 O18 Zr1'
_cod_database_code               7227807