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_7208806
_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_formula_moiety         'C38 H36 Cu2 N2 O8 P4'
_chemical_formula_sum            'C38 H36 Cu2 N2 O8 P4'
_chemical_formula_weight         899.65
_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_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   29.573(3)
_cell_length_b                   29.573(3)
_cell_length_c                   9.736(3)
_cell_measurement_reflns_used    3820
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      50.8718
_cell_measurement_theta_min      4.2099
_cell_volume                     8515(3)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
(compiled Jun 10 2008,16:49:55)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
(compiled Jun 10 2008,16:49:55)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
(compiled Jun 10 2008,16:49:55)
;
_computing_molecular_graphics    'SCHAKAL97 (Keller, 1997)'
_computing_publication_material  'PARST (Nardelli, 1995)'
_computing_structure_refinement  'SHELX (Sheldrick, 2008)'
_computing_structure_solution    'Sir97 (Altomare, 1999)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 16.4547
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur3'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0288
_diffrn_reflns_av_sigmaI/netI    0.0492
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            6935
_diffrn_reflns_theta_full        21.03
_diffrn_reflns_theta_max         21.03
_diffrn_reflns_theta_min         1.95
_exptl_absorpt_coefficient_mu    1.199
_exptl_absorpt_correction_T_max  0.9921
_exptl_absorpt_correction_T_min  0.6979
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
(compiled Jun 10 2008,16:49:55)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'pale blue'
_exptl_crystal_density_diffrn    1.404
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             3680
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.331
_refine_diff_density_min         -0.407
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.42(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     488
_refine_ls_number_reflns         4059
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0631
_refine_ls_R_factor_gt           0.0460
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0555P)^2^+32.2128P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1085
_refine_ls_wR_factor_ref         0.1166
_reflns_number_gt                3410
_reflns_number_total             4059
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ce26138c.txt
_cod_data_source_block           3
_cod_original_cell_volume        8515(2)
_cod_database_code               7208806