Crystal Engineering of a Permanently Porous Network Sustained Exclusively by Charge-Assisted Hydrogen Bonds
Sean A. Dalrymple; George K. H. Shimizu; Journal of the American Chemical Society 129 (2007) 12114–12116; doi:10.1021/ja076094v

data_4109998
_publ_contact_author_address
;University of Calgary
2500 University Drive
Calgary Alberta
T2N 1N4
;
_publ_contact_author_email       gshimizu@ucalgary.ca
_publ_contact_author_name        G.K.H.Shimizu
_publ_section_title
;
 Crystal Engineering of a Permanently Porous Network Sustained Exclusively
 by Charge-Assisted Hydrogen Bonds
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12114
_journal_page_last               12116
_journal_paper_doi               10.1021/ja076094v
_journal_volume                  129
_journal_year                    2007
_chemical_formula_moiety         'C10 H29.94 N6 Ni, 2(C8 H5 O3 S)'
_chemical_formula_sum            'C26 H39.94 N6 Ni O6 S2'
_chemical_formula_weight         655.41
_chemical_name_common            '[Ni(tame)2]1(PES)2'
_chemical_name_systematic
; 
 bis(1,1,1-tris(aminomethyl)ethane)nickel(II)di(2-phenylethynesulfonate) 
;
_space_group_IT_number           147
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      147
_symmetry_space_group_name_Hall  '-P 3'
_symmetry_space_group_name_H-M   'P -3'
_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                120.00
_cell_formula_units_Z            3
_cell_length_a                   13.862(5)
_cell_length_b                   13.862(5)
_cell_length_c                   13.784(5)
_cell_measurement_reflns_used    3488
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.39
_cell_volume                     2293.8(14)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'HKL Denzo and Scalepack'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0318
_diffrn_reflns_av_sigmaI/netI    0.0431
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            6703
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.39
_exptl_absorpt_coefficient_mu    0.820
_exptl_absorpt_correction_T_max  0.8869
_exptl_absorpt_correction_T_min  0.8402
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Sheldrick 2002)'
_exptl_crystal_colour            Purple
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1037.8
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.303
_refine_diff_density_min         -0.624
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         3488
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0689
_refine_ls_R_factor_gt           0.0398
_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^)+(0.0569P)^2^+0.0358P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0989
_refine_ls_wR_factor_ref         0.1127
_reflns_number_gt                2444
_reflns_number_total             3488
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja076094vsi20070817_075835.cif
_cod_data_source_block           import
_cod_database_code               4109998