Helicates, Boxes, and Polymers from Simple Pyridine-Alcohol Ligands: the Impact of the Identity of the Transition Metal Ion
Shane G. Telfer; Nyree D. Parker; Reiko Kuroda; Takunori Harada; Julie Lefebvre; Daniel B. Leznoff; Inorganic Chemistry 47 (2008) 209–218; doi:10.1021/ic701757e

data_4304285
_publ_section_title
;
Helicates, Boxes, and Polymers from Simple Pyridine-Alcohol Ligands: the
Impact of the Identity of the Transition Metal Ion
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              209
_journal_page_last               218
_journal_paper_doi               10.1021/ic701757e
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C69 H96 Cl4 N8 Ni8 O21'
_chemical_formula_weight         1985.02
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_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                   15.9492(13)
_cell_length_b                   35.895(3)
_cell_length_c                   13.9089(11)
_cell_measurement_reflns_used    9999
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.92
_cell_measurement_theta_min      1.40
_cell_volume                     7962.8(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_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  0.0439
_diffrn_reflns_av_sigmaI/netI    0.0689
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            47874
_diffrn_reflns_theta_full        27.92
_diffrn_reflns_theta_max         27.92
_diffrn_reflns_theta_min         1.40
_exptl_absorpt_coefficient_mu    2.058
_exptl_absorpt_correction_T_max  0.8207
_exptl_absorpt_correction_T_min  0.6272
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.656
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4104
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.638
_refine_diff_density_min         -0.733
_refine_diff_density_rms         0.133
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    fixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1002
_refine_ls_number_reflns         18174
_refine_ls_number_restraints     440
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0776
_refine_ls_R_factor_gt           0.0575
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0607P)^2^+17.9916P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1320
_refine_ls_wR_factor_ref         0.1391
_reflns_number_gt                14121
_reflns_number_total             18174
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic701757e-file012_7.cif
_cod_data_source_block           '[Ni4(1-H)4(OAc)2Cl2(MeOH)2]'
_cod_database_code               4304285