A Water and Thermally Stable Metal‒Organic Framework Featuring Selective CO2Adsorption
Li, Yameng; Ju, Zhanfeng; Wu, Benlai; Yuan, Daqiang; Crystal Growth & Design 13 (2013) 4125–; doi:10.1021/cg400948e

data_4508265
_publ_section_title
;
 A Water and Thermally Stable Metal--Organic Framework Featuring Selective
 CO2Adsorption
;
_journal_issue                   9
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              4125
_journal_paper_doi               10.1021/cg400948e
_journal_volume                  13
_journal_year                    2013
_chemical_formula_moiety         'C34 H20 N6 Ni2 O8'
_chemical_formula_sum            'C34 H20 N6 Ni2 O8'
_chemical_formula_weight         757.98
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 116.608(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.513(3)
_cell_length_b                   22.317(3)
_cell_length_c                   11.6320(15)
_cell_measurement_reflns_used    2870
_cell_measurement_temperature    433.00(10)
_cell_measurement_theta_max      72.5880
_cell_measurement_theta_min      3.9490
_cell_volume                     4528.9(13)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      433.00(10)
_diffrn_detector_area_resol_mean 10.5594
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0244
_diffrn_reflns_av_unetI/netI     0.0299
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.949
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8588
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.949
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.157
_diffrn_reflns_theta_min         4.251
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.418
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87082
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.112
_exptl_crystal_description       prism
_exptl_crystal_F_000             1544
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.030
_platon_squeeze_details
;
There are one-dimension channels in this complex,
in which some disordered water molecules exist at the low temperature 
(100 K).However, at high temperature (433 K) these disordered water 
molecules are removed completely.Thus, there is a large solvent 
accessible void. In order to compare this high temperature framework 
with that at 100 K using the 'SQUEEZE' instruction, 
we use the 'SQUEEZE' instruction again. 
;
_refine_diff_density_max         0.823
_refine_diff_density_min         -0.273
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     229
_refine_ls_number_reflns         4436
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0643
_refine_ls_R_factor_gt           0.0541
_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^)+(0.0964P)^2^+3.0453P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1636
_refine_ls_wR_factor_ref         0.1703
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3537
_reflns_number_total             4436
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cg400948e_si_002.cif
_cod_data_source_block           complex1-433K-sq
_cod_original_cell_volume        4529.1(12)
_cod_database_code               4508265
_shelx_estimated_absorpt_t_min   0.895
_shelx_estimated_absorpt_t_max   0.959