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_7227809
_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, 2(C H8 N4 S), 2(H2 O)'
_chemical_formula_sum            'C10 H20 N8 O18 S2 Zr'
_chemical_formula_weight         695.66
_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     other
_audit_update_record
;
2016-11-09 deposited with the CCDC.
2017-02-17 downloaded from the CCDC.
;
_cell_angle_alpha                78.14(3)
_cell_angle_beta                 89.23(5)
_cell_angle_gamma                86.71(3)
_cell_formula_units_Z            2
_cell_length_a                   10.077(9)
_cell_length_b                   10.810(10)
_cell_length_c                   11.116(11)
_cell_measurement_reflns_used    8654
_cell_measurement_temperature    100
_cell_measurement_theta_max      35
_cell_measurement_theta_min      4
_cell_volume                     1183.1(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    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.918
_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  0.032
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            39412
_diffrn_reflns_theta_full        25.334
_diffrn_reflns_theta_max         34.703
_diffrn_reflns_theta_min         1.872
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.744
_exptl_absorpt_correction_T_max  0.86
_exptl_absorpt_correction_T_min  0.78
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.953
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             704
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         3.16
_refine_diff_density_min         -1.29
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.8618
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         7487
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0566
_refine_ls_R_factor_gt           0.0488
_refine_ls_shift/su_max          0.0013993
_refine_ls_shift/su_mean         0.0000385
_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: 
 0.426 0.424 0.226 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0469
_refine_ls_wR_factor_gt          0.0409
_refine_ls_wR_factor_ref         0.0402
_reflns_limit_h_max              16
_reflns_limit_h_min              -16
_reflns_limit_k_max              17
_reflns_limit_k_min              -16
_reflns_limit_l_max              17
_reflns_limit_l_min              0
_reflns_number_gt                8001
_reflns_number_total             9351
_reflns_threshold_expression     I>2.0\s(I)
_oxford_refine_ls_r_factor_ref   0.0470
_oxford_reflns_number_all        9333
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            c6ce02547a2.cif
_cod_data_source_block           cpd1
_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        1183.0(12)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C10 H20 N8 O18 S2 Zr1'
_cod_database_code               7227809