A Metal-Organic Bilayer Open Framework with a Dynamic Component: Single-Crystal-to-Single-Crystal Transformations
Myunghyun Paik Suh; Jung Woo Ko; Hye Jin Choi; Journal of the American Chemical Society 124 (2002) 10976–10977; doi:10.1021/ja017560y

data_4115136
_publ_section_title
;
 A Metal-Organic Bilayer Open Framework with a Dynamic Component:
 Single-Crystal-to-Single-Crystal Transformations
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10976
_journal_page_last               10977
_journal_paper_doi               10.1021/ja017560y
_journal_volume                  124
_journal_year                    2002
_chemical_formula_sum            'C99 H145 N15 Ni3 O21.5'
_chemical_formula_weight         2065.43
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                70.498(5)
_cell_angle_beta                 71.084(5)
_cell_angle_gamma                76.297(5)
_cell_formula_units_Z            2
_cell_length_a                   16.460(5)
_cell_length_b                   19.849(5)
_cell_length_c                   20.419(5)
_cell_measurement_temperature    293(2)
_cell_volume                     5887(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.696
_diffrn_measured_fraction_theta_max 0.696
_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  0.1444
_diffrn_reflns_av_sigmaI/netI    0.6290
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            22387
_diffrn_reflns_theta_full        25.75
_diffrn_reflns_theta_max         25.75
_diffrn_reflns_theta_min         1.10
_exptl_absorpt_coefficient_mu    0.541
_exptl_crystal_density_diffrn    1.165
_exptl_crystal_F_000             2200
_refine_diff_density_max         0.670
_refine_diff_density_min         -0.525
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.943
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1031
_refine_ls_number_reflns         15661
_refine_ls_number_restraints     1008
_refine_ls_restrained_S_all      0.920
_refine_ls_R_factor_all          0.4091
_refine_ls_R_factor_gt           0.1299
_refine_ls_shift/su_max          6.933
_refine_ls_shift/su_mean         0.122
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3464
_refine_ls_wR_factor_ref         0.4543
_reflns_number_gt                3439
_reflns_number_total             15661
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja017560y_s2_6.cif
_cod_data_source_block           Ni2(C26H52N10)]3[BTC]4.14C6H6.19H2O
_cod_original_formula_sum        'C99 H145 N15 Ni3 O21.50'
_cod_database_code               4115136