Porous Coordination Polymer Based on Bipyridinium Carboxylate Linkers with High and Reversible Ammonia Uptake.
Leroux, Maxime; Mercier, Nicolas; Allain, Magali; Dul, Marie-Claire; Dittmer, Jens; Kassiba, Abdel Hadi; Bellat, Jean-Pierre; Weber, Guy; Bezverkhyy, Igor; Inorganic chemistry 55 (2016) 8587–8594; doi:10.1021/acs.inorgchem.6b01119

data_4348346
_publ_section_title
;
 Porous Coordination Polymer Based on Bipyridinium Carboxylate Linkers
 with High and Reversible Ammonia Uptake.
;
_journal_issue                   17
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8587
_journal_page_last               8594
_journal_paper_doi               10.1021/acs.inorgchem.6b01119
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C72 H64 Cd5 Cl10 N6 O20'
_chemical_formula_sum            'C72 H64 Cd5 Cl10 N6 O20'
_chemical_formula_weight         2249.79
_space_group_IT_number           163
_space_group_name_Hall           '-P 3 2c'
_space_group_name_H-M_alt        'P -3 1 c'
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'P -3 1 c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000
_cell_angle_beta                 90.000
_cell_angle_gamma                120.000
_cell_formula_units_Z            2
_cell_length_a                   18.196(5)
_cell_length_b                   18.196(5)
_cell_length_c                   15.127(5)
_cell_measurement_reflns_used    15567
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      75.7950
_cell_measurement_theta_min      4.0170
_cell_volume                     4337(2)
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      180(2)
_diffrn_detector_area_resol_mean 5.1990
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'SuperNova, Single source at offset, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0299
_diffrn_reflns_av_sigmaI/netI    0.0135
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            27801
_diffrn_reflns_theta_full        76.53
_diffrn_reflns_theta_max         76.53
_diffrn_reflns_theta_min         2.80
_exptl_absorpt_coefficient_mu    13.074
_exptl_absorpt_correction_T_max  0.3547
_exptl_absorpt_correction_T_min  0.1529
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.723
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2216
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
The unit cell contains disordered water molecules which were
not modelled but the corresponding scattering contribution
were taken into account using SQUEEZE/PLATON procedure.
The unit cell contains 1 void of 346 A3 containing about
94 electrons which corresponds to approximately 8 water
molecules . The solvent composition was included in
the calculation of the empirical formula, formula weight,
density, linear absorption coefficient and F(000).
;
_refine_diff_density_max         0.649
_refine_diff_density_min         -0.723
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     175
_refine_ls_number_reflns         3027
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_gt           0.0391
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0483P)^2^+5.2851P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0972
_refine_ls_wR_factor_ref         0.1022
_reflns_number_gt                2626
_reflns_number_total             3027
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b01119_si_002.cif
_cod_data_source_block           hexagonal
_cod_original_sg_symbol_H-M      P-31C
_cod_database_code               4348346