Solvent dependent synthesis of micro- and nano- crystalline phosphinate based 1D tubular MOF: structure and CO2 adsorption selectivity
Bataille, Thierry; Bracco, Silvia; Comotti, Angiolina; Costantino, Ferdinando; Guerri, Annalisa; Ienco, Andrea; Marmottini, Fabio; CrystEngComm 14 (2012) 7170–; doi:10.1039/c2ce26138c

data_7208805
_publ_section_title
;
 Solvent dependent synthesis of micro- and nano- crystalline phosphinate
 based 1D tubular MOF: structure and CO2 adsorption selectivity
;
_journal_issue                   21
_journal_name_full               CrystEngComm
_journal_page_first              7170
_journal_paper_doi               10.1039/c2ce26138c
_journal_volume                  14
_journal_year                    2012
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C38 H38 Cu2 N2 O9 P4'
_chemical_formula_sum            'C38 H38 Cu2 N2 O9 P4'
_chemical_formula_weight         917.66
_chemical_name_systematic
;
?
;
_space_group_IT_number           82
_symmetry_cell_setting           tetragonal
_symmetry_Int_Tables_number      82
_symmetry_space_group_name_Hall  'I -4'
_symmetry_space_group_name_H-M   'I -4'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2011-05-18 # Formatted by publCIF
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   29.610(4)
_cell_length_b                   29.610(4)
_cell_length_c                   9.770(2)
_cell_measurement_reflns_used    1067
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      50.7269
_cell_measurement_theta_min      4.2125
_cell_volume                     8566(2)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May 6 2009,17:20:42)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May 6 2009,17:20:42)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May 6 2009,17:20:42)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 8.1241
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Xcalibur, Onyx'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.031895323
_diffrn_orient_matrix_UB_12      0.0361438844
_diffrn_orient_matrix_UB_13      -0.060883015
_diffrn_orient_matrix_UB_21      -0.0382463338
_diffrn_orient_matrix_UB_22      0.0352844575
_diffrn_orient_matrix_UB_23      0.0084219059
_diffrn_orient_matrix_UB_31      0.0153834875
_diffrn_orient_matrix_UB_32      0.0129036998
_diffrn_orient_matrix_UB_33      0.1457094996
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.081
_diffrn_reflns_av_unetI/netI     0.2148
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            7721
_diffrn_reflns_theta_full        51.03
_diffrn_reflns_theta_max         51.03
_diffrn_reflns_theta_min         4.22
_exptl_absorpt_coefficient_mu    3.08
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.66725
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May 6 2009,17:20:42)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light blue'
_exptl_crystal_density_diffrn    1.423
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             3760
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.411
_refine_diff_density_min         -0.562
_refine_diff_density_rms         0.11
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.09(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.991
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     267
_refine_ls_number_reflns         4301
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.2049
_refine_ls_R_factor_gt           0.0798
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1074P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1724
_refine_ls_wR_factor_ref         0.226
_reflns_number_gt                2069
_reflns_number_total             4301
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ce26138c.txt
_cod_data_source_block           1
_cod_database_code               7208805