Chiral Direction and Interconnection of Helical Three-Connected Networks in Metal-Organic Frameworks
T. J. Prior; M. J. Rosseinsky; Inorganic Chemistry 42 (2003) 1564–1575; doi:10.1021/ic025775i

data_4313268
_publ_contact_author
;
      Matthew J Rosseinsky
      Department of Chemistry
      The University of Liverpool
      Liverpool
      L69 7ZD
      UK
;
_publ_contact_author_email       m.j.rosseinsky@liv.ac.uk
_publ_contact_author_fax         '(44) 151 794 3587'
_publ_contact_author_phone       '(44) 151 794 3499'
_publ_section_title
;
 Chiral Direction and Interconnection of Helical Three-Connected Networks
 in Metal-Organic Frameworks
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1564
_journal_page_last               1575
_journal_paper_doi               10.1021/ic025775i
_journal_volume                  42
_journal_year                    2003
_chemical_formula_structural
; 'Ni 3 (C9 H 3 O 6) 2 (C 5 H 5 N) 6 (C 4 H 10 O 2) 4 (mu-C 4 H 10 O 2) 
. 2(C 4 H 10 O 2)'
;
_chemical_formula_sum            'C72 H42 N6 Ni3 O24'
_chemical_formula_weight         1551.33
_chemical_name_systematic
; 
Ni1.5(btc)(py)3(14bd)3(14bd)
;
_space_group_IT_number           95
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4cw 2c'
_symmetry_space_group_name_H-M   'P 43 2 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            4
_cell_length_a                   16.3116(14)
_cell_length_b                   16.3116(14)
_cell_length_c                   30.060(3)
_cell_measurement_reflns_used    6445
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      24.31
_cell_measurement_theta_min      1.77
_cell_volume                     7998.0(13)
_computing_cell_refinement       'Stoe IPDS system'
_computing_data_collection       'Stoe IPDS system'
_computing_data_reduction        'Stoe IPDS system'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Stoe IPDS diffractometer'
_diffrn_measurement_method       '100 2 degree oscillations in phi'
_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  0.1912
_diffrn_reflns_av_sigmaI/netI    0.1999
_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       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            51862
_diffrn_reflns_theta_full        24.31
_diffrn_reflns_theta_max         24.31
_diffrn_reflns_theta_min         1.77
_exptl_absorpt_coefficient_mu    0.721
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       octahedron
_exptl_crystal_F_000             3167
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.840
_refine_diff_density_min         -0.324
_refine_diff_density_rms         0.087
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.785
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     421
_refine_ls_number_reflns         6445
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      0.789
_refine_ls_R_factor_all          0.1400
_refine_ls_R_factor_gt           0.0641
_refine_ls_shift/su_max          0.054
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0799P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1440
_refine_ls_wR_factor_ref         0.1672
_reflns_number_gt                2873
_reflns_number_total             6445
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic025775isi20021029_111527_1.cif
_cod_data_source_block           Prior1
_cod_original_cell_volume        7998.1(13)
_cod_database_code               4313268