Helicity Induction through Hydrogen Bonding and Spontaneous Resolution of a Bimetallic Nickel Complex Coordinated to an Octahedral Metalloligand
Khatua, Snehadrinarayan; Stoeckli-Evans, Helen; Harada, Takunori; Kuroda, Reiko; Bhattacharjee, Manish; Inorganic Chemistry 45 (2006) 9619–9621; doi:10.1021/ic061226r

data_4332994
_publ_section_title
;
 Helicity Induction through Hydrogen Bonding and Spontaneous Resolution of
 a Bimetallic Nickel Complex Coordinated to an Octahedral Metalloligand
;
_journal_issue                   24
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9619
_journal_page_last               9621
_journal_paper_doi               10.1021/ic061226r
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C40 H71 Mo2 N2 Ni O21.5'
_chemical_formula_weight         1174.58
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 96.355(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.6309(11)
_cell_length_b                   11.5596(7)
_cell_length_c                   16.6061(12)
_cell_measurement_reflns_used    30861
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.64
_cell_measurement_theta_min      1.34
_cell_volume                     2600.5(3)
_computing_cell_refinement       'X-Area V1.26'
_computing_data_collection       'X-Area V1.26 (STOE, 2005)'
_computing_data_reduction        'X-RED32 V1.26 (STOE, 2005)'
_computing_molecular_graphics    'PLATON  (Spek, 2003)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'STOE IPDS-2'
_diffrn_measurement_method       'omega scans'
_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  0.0594
_diffrn_reflns_av_sigmaI/netI    0.0536
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            36704
_diffrn_reflns_theta_full        29.39
_diffrn_reflns_theta_max         29.39
_diffrn_reflns_theta_min         1.84
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.908
_exptl_absorpt_correction_T_max  0.644
_exptl_absorpt_correction_T_min  0.172
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'DIFrelABS in PLATON; Spek, 2003)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.500
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1218
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.487
_refine_diff_density_min         -1.480
_refine_diff_density_rms         0.098
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.03(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     619
_refine_ls_number_reflns         14013
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0639
_refine_ls_R_factor_gt           0.0519
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         <0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0621P)^2^+3.5057P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1239
_refine_ls_wR_factor_ref         0.1323
_reflns_number_gt                12092
_reflns_number_total             14013
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ic061226rsup1.cif
_cod_data_source_block           1a
_cod_original_sg_symbol_H-M      'P 21'
_cod_original_formula_sum        'C40 H71 Mo2 N2 Ni O21.50'
_cod_database_code               4332994