In Situ Single-Crystal X-ray Diffraction Studies of Desorption and Sorption in a Flexible Nanoporous Molecular Framework Material
Gregory J. Halder; Cameron J. Kepert; Journal of the American Chemical Society 127 (2005) 7891–7900; doi:10.1021/ja042420k

data_4111701
_publ_contact_author
;
 Cameron J. Kepert
 School of Chemistry, F11
 University of Sydney
 NSW 2006
 Australia
;
_publ_contact_author_email       c.kepert@chem.usyd.edu.au
_publ_contact_author_fax         +61-2-9351-3329
_publ_contact_author_phone       +61-2-9351-5741
_publ_section_title
;
 In Situ Single-Crystal X-ray Diffraction Studies of Desorption and
 Sorption in a Flexible Nanoporous Molecular Framework Material
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7891
_journal_page_last               7900
_journal_paper_doi               10.1021/ja042420k
_journal_volume                  127
_journal_year                    2005
_chemical_formula_moiety         'C14 H12 Co N5 O6, C5 H8 O'
_chemical_formula_sum            'C19 H20 Co N5 O7'
_chemical_formula_weight         489.33
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           68
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      68
_symmetry_space_group_name_Hall  '-C 2a 2ac'
_symmetry_space_group_name_H-M   'C c c a :2'
_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                   13.116(5)
_cell_length_b                   19.085(7)
_cell_length_c                   17.934(7)
_cell_measurement_reflns_used    938
_cell_measurement_temperature    310(2)
_cell_measurement_theta_max      26.799
_cell_measurement_theta_min      2.200
_cell_volume                     4489(3)
_computing_cell_refinement       'SMART (BrukerAXS, 1997)'
_computing_data_collection       'SMART (BrukerAXS, 1997)'
_computing_data_reduction        'SAINT+ (BrukerAXS, 1997)'
_computing_molecular_graphics    'XPMA/ZORTEP, WebLab Viewer 3.7'
_computing_publication_material  XCIF
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      310(2)
_diffrn_measured_fraction_theta_full 0.952
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0461
_diffrn_reflns_av_sigmaI/netI    0.0330
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            20360
_diffrn_reflns_theta_full        28.02
_diffrn_reflns_theta_max         28.02
_diffrn_reflns_theta_min         2.13
_diffrn_standards_decay_%        0.00
_diffrn_standards_number         131
_exptl_absorpt_coefficient_mu    0.814
_exptl_absorpt_correction_T_max  0.783
_exptl_absorpt_correction_T_min  0.418
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS, Bruker 1995'
_exptl_crystal_colour            purple-red
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_description       block-shaped
_exptl_crystal_F_000             2016
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.353
_refine_diff_density_min         -0.881
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     132
_refine_ls_number_reflns         2594
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.1295
_refine_ls_R_factor_gt           0.0944
_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^)+(0.1457P)^2^+22.0816P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2571
_refine_ls_wR_factor_ref         0.2962
_reflns_number_gt                1758
_reflns_number_total             2594
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja042420ksi20041217_015043.cif
_cod_data_source_block           1.(THF)
_cod_original_sg_symbol_Hall     '-C 2b 2bc'
_cod_original_sg_symbol_H-M      'C c c a'
_cod_database_code               4111701