Supramolecular open-framework architectures based on dicarboxylate H-bond acceptors and polytopic cations with three/four N–H+donor units
Mouchaham, Georges; Gualino, Marion; Roques, Nans; Duhayon, Carine; Brandès, Stéphane; Sutter, Jean-Pascal; CrystEngComm 17 (2015) 8906–; doi:10.1039/C5CE01070E

data_7221682
_publ_section_title
;
 Supramolecular open-framework architectures based on dicarboxylate H-bond
 acceptors and polytopic cations with three/four N--H+donor units
;
_journal_issue                   46
_journal_name_full               CrystEngComm
_journal_page_first              8906
_journal_paper_doi               10.1039/C5CE01070E
_journal_volume                  17
_journal_year                    2015
_chemical_formula_moiety         'C15 H15 N6, C2 O4, C2 H O4, 5(H2 O)'
_chemical_formula_sum            'C19 H26 N6 O13'
_chemical_formula_weight         546.45
_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     other
_audit_update_record
;
2015-05-21 deposited with the CCDC.
2015-07-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.565(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.3011(4)
_cell_length_b                   24.6348(6)
_cell_length_c                   7.1285(2)
_cell_measurement_reflns_used    11820
_cell_measurement_temperature    180
_cell_measurement_theta_max      72
_cell_measurement_theta_min      3
_cell_volume                     2320.48(11)
_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    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      180
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction Gemini'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.022
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            23350
_diffrn_reflns_theta_full        71.763
_diffrn_reflns_theta_max         71.763
_diffrn_reflns_theta_min         3.345
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.158
_exptl_absorpt_correction_T_max  0.94
_exptl_absorpt_correction_T_min  0.69
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.564
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       planar
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.35
_refine_diff_density_min         -0.28
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0385
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         4185
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_gt           0.0358
_refine_ls_shift/su_max          0.0007884
_refine_ls_shift/su_mean         0.0000845
_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: 
 5.16 1.93 3.39 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0426
_refine_ls_wR_factor_gt          0.0417
_refine_ls_wR_factor_ref         0.0413
_reflns_limit_h_max              16
_reflns_limit_h_min              -16
_reflns_limit_k_max              30
_reflns_limit_k_min              0
_reflns_limit_l_max              8
_reflns_limit_l_min              0
_reflns_number_gt                4291
_reflns_number_total             4532
_reflns_threshold_expression     I>2.0\s(I)
_oxford_refine_ls_r_factor_ref   0.0349
_oxford_reflns_number_all        4512
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_iucr_refine_instructions_details_constraints
;
BLOCK SCALE X'S, U'S 
RIDE C   (   2,X'S) H   (  21,X'S) 
RIDE C   (   4,X'S) H   (  41,X'S) 
RIDE C   (   6,X'S) H   (  61,X'S) 
RIDE C   (   8,X'S) H   (  81,X'S) 
RIDE N   (   9,X'S) H   (  91,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) 
RIDE N   (  14,X'S) H   ( 141,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) 
RIDE C   (  18,X'S) H   ( 181,X'S) 
RIDE N   (  19,X'S) H   ( 191,X'S) 
RIDE C   (  20,X'S) H   ( 201,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) 
RIDE O   (  33,X'S) H   ( 331,X'S) 
RIDE O   (  34,X'S) H   ( 342,X'S) H   ( 341,X'S) 
RIDE O   (  35,X'S) H   ( 352,X'S) H   ( 351,X'S) 
RIDE O   (  36,X'S) H   ( 362,X'S) H   ( 361,X'S) 
RIDE O   (  37,X'S) H   ( 371,X'S) H   ( 372,X'S) 
RIDE O   (  38,X'S) H   ( 382,X'S) H   ( 381,X'S) 
END                                                                             
;
_iucr_refine_instructions_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
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_cod_data_source_file            c5ce01070e2.cif
_cod_data_source_block           cpd3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Other' changed to 'other'
according to
/usr/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 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 7221680--7221684.cif.
;
_cod_original_cell_volume        2320.50(12)
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_database_code               7221682