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_7221681
_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         'C25 H28 N4 O4, 2(C6 Cl2 O4), 3(C3 H7 N O)'
_chemical_formula_sum            'C46 H49 Cl4 N7 O15'
_chemical_formula_weight         1081.74
_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
;
2015-05-21 deposited with the CCDC.
2015-07-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 114.8000(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.72290(10)
_cell_length_b                   34.3062(4)
_cell_length_c                   15.2099(2)
_cell_measurement_reflns_used    26937
_cell_measurement_temperature    180
_cell_measurement_theta_max      62
_cell_measurement_theta_min      3
_cell_volume                     5079.15(11)
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_collection       'Gemini, (Oxford Diffraction, 2006)'
_computing_data_reduction        'XRED (Stoe & Cie 1996)'
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.026
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            41877
_diffrn_reflns_theta_full        62.027
_diffrn_reflns_theta_max         62.027
_diffrn_reflns_theta_min         3.450
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.748
_exptl_absorpt_correction_T_max  0.65
_exptl_absorpt_correction_T_min  0.41
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.415
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2248
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         1.48
_refine_diff_density_min         -0.87
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9676
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     649
_refine_ls_number_reflns         7130
_refine_ls_number_restraints     72
_refine_ls_R_factor_all          0.0747
_refine_ls_R_factor_gt           0.0716
_refine_ls_shift/su_max          0.0008338
_refine_ls_shift/su_mean         0.0000379
_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: 
 15.6 14.8 12.8 3.87 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0873
_refine_ls_wR_factor_gt          0.0864
_refine_ls_wR_factor_ref         0.0861
_reflns_limit_h_max              11
_reflns_limit_h_min              -12
_reflns_limit_k_max              39
_reflns_limit_k_min              0
_reflns_limit_l_max              17
_reflns_limit_l_min              0
_reflns_number_gt                7409
_reflns_number_total             7995
_reflns_threshold_expression     I>2.0\s(I)
_oxford_refine_ls_r_factor_ref   0.0698
_oxford_reflns_number_all        7957
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            c5ce01070e2.cif
_cod_data_source_block           Cpd2
_cod_depositor_comments
'Adding full bibliography for 7221680--7221684.cif.'
_cod_original_sg_symbol_Hall     '-P 2ybc '
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_database_code               7221681
_iucr_refine_instructions_details_constraints
;
BLOCK SCALE X'S, U'S 
RIDE N   (   7,X'S) H   (  71,X'S) 
RIDE N   (  15,X'S) H   ( 151,X'S) 
RIDE N   (  23,X'S) H   ( 231,X'S) 
RIDE N   (  31,X'S) H   ( 311,X'S) 
RIDE C   (   2,X'S) H   (  22,X'S) H   (  21,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) 
RIDE C   (   6,X'S) H   (  61,X'S) 
RIDE C   (   8,X'S) H   (  81,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) 
RIDE C   (  10,X'S) H   ( 102,X'S) H   ( 101,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) 
RIDE C   (  17,X'S) H   ( 171,X'S) 
RIDE C   (  18,X'S) H   ( 182,X'S) H   ( 181,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) 
RIDE C   (  26,X'S) H   ( 261,X'S) H   ( 262,X'S) 
RIDE C   (  29,X'S) H   ( 291,X'S) 
RIDE C   (  30,X'S) H   ( 301,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) 
RIDE C   (  47,X'S) H   ( 471,X'S) 
RIDE C   (  49,X'S) H   ( 493,X'S) H   ( 492,X'S) H   ( 491,X'S) 
RIDE C   (  50,X'S) H   ( 503,X'S) H   ( 502,X'S) H   ( 501,X'S) 
RIDE C   (  52,X'S) H   ( 521,X'S) 
RIDE C   (  54,X'S) H   ( 543,X'S) H   ( 541,X'S) H   ( 542,X'S) 
RIDE C   (  55,X'S) H   ( 551,X'S) H   ( 553,X'S) H   ( 552,X'S) 
RIDE C   (  57,X'S) H   ( 571,X'S) 
RIDE C   (  59,X'S) H   ( 592,X'S) H   ( 593,X'S) H   ( 591,X'S) 
RIDE C   (  60,X'S) H   ( 603,X'S) H   ( 602,X'S) H   (6031,X'S) 
END                                                                             
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_iucr_refine_instructions_details_restraints
;
DELU   .005 O(51)  C(52)  N(53) C(54) C(55) 
CONT AND O(56)  C(57)  N(58) C(59) C(60) 
SIMU   .005 O(51)  C(52)  N(53) C(54) C(55) 
CONT AND O(56)  C(57)  N(58) C(59) C(60) 
SAME  O(51)  C(52)  N(53) C(54) C(55) 
CONT AND O(56)  C(57)  N(58) C(59) C(60) 
U(IJ) 0,.005 = O(51)TO O(56), C(52) TO C(57) , 
CONT N(53) TO C(58), C(54) TO C(59), C(55) TO C(60) 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
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