Hierarchical Helix of Helix in the Crystal: Formation of Variable-Pitch Helical π-Stacked Array of Single-Helical Dinuclear Metal Complexes
Shigehisa Akine; Hiroki Nagumo; Tatsuya Nabeshima; Inorganic Chemistry 51 (2012) 5506–5508; doi:10.1021/ic3004273

data_4329230
_publ_contact_author_address
;
Tsukuba, Ibaraki 305-8571, Japan
;
_publ_contact_author_email       akine@chem.tsukuba.ac.jp
_publ_contact_author_fax         +81-29-853-4527
_publ_contact_author_name        'Shigehisa Akine'
_publ_contact_author_phone       +81-29-853-4527
_publ_section_title
;
 Hierarchical Helix of Helix in the Crystal: Formation of Variable-Pitch
 Helical \p-Stacked Array of Single-Helical Dinuclear Metal Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5506
_journal_page_last               5508
_journal_paper_doi               10.1021/ic3004273
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         C72.50H70.50N7.20Ni2O9.35
_chemical_formula_sum            'C72.5 H70.5 N7.2 Ni2 O9.35'
_chemical_formula_weight         1309.68
_chemical_name_common            '[LNi2]_3.2DMF_0.15iPr2O'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_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                 90.5890(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            12
_cell_length_a                   22.1467(6)
_cell_length_b                   27.5484(8)
_cell_length_c                   31.0547(8)
_cell_measurement_reflns_used    167384
_cell_measurement_temperature    120
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      1.48
_cell_volume                     18945.7(9)
_computing_cell_refinement       'APEX2 (Bruker AXS, 2009)'
_computing_data_collection       'APEX2 (Bruker AXS, 2009)'
_computing_data_reduction        'APEX2 (Bruker AXS, 2009)'
_computing_molecular_graphics    ORTEP-3
_computing_publication_material  ORTEP-3
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXD (Sheldrick, 2000)'
_diffrn_ambient_temperature      120
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'multilayer confocal mirror'
_diffrn_radiation_source         'fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0397
_diffrn_reflns_av_sigmaI/netI    0.0446
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            167384
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.48
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.663
_exptl_absorpt_correction_T_max  0.8789
_exptl_absorpt_correction_T_min  0.8260
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.377
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             8240
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.742
_refine_diff_density_min         -0.671
_refine_diff_density_rms         0.076
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.022(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2438
_refine_ls_number_reflns         43405
_refine_ls_number_restraints     174
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0574
_refine_ls_R_factor_gt           0.0489
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0868P)^2^+16.0286P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1312
_refine_ls_wR_factor_ref         0.1377
_reflns_number_gt                38729
_reflns_number_total             43405
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3004273_si_003.cif
_cod_data_source_block           nag372
_cod_original_formula_sum        'C72.50 H70.50 N7.20 Ni2 O9.35'
_cod_database_code               4329230