Kinetic molecular sieving, thermodynamic and structural aspects of gas/vapor sorption on metal organic framework [Ni1.5(4,4′-bipyridine)1.5(H3L)(H2O)3][H2O]7 where H6L = 2,4,6-trimethylbenzene-1,3,5-triyl tris(methylene)triphosphonic acid
Zhao, Xuebo; Bell, Jon G.; Tang, Si-Fu; Li, Liangjun; Thomas, K. Mark; Journal of Materials Chemistry A 4 (2016) 1353–; doi:10.1039/C5TA08261G

data_7236124
_publ_section_title
;
 Kinetic molecular sieving, thermodynamic and structural aspects of
 gas/vapor sorption on metal organic framework
 [Ni1.5(4,4&#x2032;-bipyridine)1.5(H3L)(H2O)3][H2O]7 where H6L =
 2,4,6-trimethylbenzene-1,3,5-triyl tris(methylene)triphosphonic acid
;
_journal_issue                   4
_journal_name_full               'Journal of Materials Chemistry A'
_journal_page_first              1353
_journal_paper_doi               10.1039/C5TA08261G
_journal_volume                  4
_journal_year                    2016
_chemical_formula_sum            'C27 H36.5 N3 Ni1.5 O12.25 P3'
_chemical_formula_weight         780.06
_space_group_crystal_system      tetragonal
_space_group_IT_number           121
_space_group_name_Hall           'I -4 2'
_space_group_name_H-M_alt        'I -4 2 m'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2015-09-18 deposited with the CCDC.
2015-12-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.5126(12)
_cell_length_b                   18.5126(12)
_cell_length_c                   22.922(3)
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.559
_cell_measurement_theta_min      1.414
_cell_volume                     7855.7(13)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0567
_diffrn_reflns_av_unetI/netI     0.1020
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            14573
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.559
_diffrn_reflns_theta_min         1.414
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.904
_exptl_absorpt_correction_T_max  0.835
_exptl_absorpt_correction_T_min  0.729
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.319
_exptl_crystal_description       colum
_exptl_crystal_F_000             3236
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.611
_refine_diff_density_min         -0.466
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details
;
 Flack x determined using 779 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.028(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.857
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     231
_refine_ls_number_reflns         4617
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      0.862
_refine_ls_R_factor_all          0.1179
_refine_ls_R_factor_gt           0.0585
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0800P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1313
_refine_ls_wR_factor_ref         0.1468
_reflns_Friedel_coverage         0.817
_reflns_Friedel_fraction_full    0.980
_reflns_Friedel_fraction_max     0.958
_reflns_number_gt                2231
_reflns_number_total             4617
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ta08261g2.cif
_cod_data_source_block           activated
_cod_original_cell_volume        7855.6(15)
_cod_original_formula_sum        'C27 H36.50 N3 Ni1.50 O12.25 P3'
_cod_database_code               7236124
_shelxl_version_number           2013-2
_shelx_res_checksum              49861
_shelx_hkl_checksum              41247