Spontaneous Resolution of a New Thiogermanate Containing Chiral Binuclear Nickel(II) Complexes with Achiral Triethylenetetramine Ligands: A Unique Water-Mediated Supramolecular Hybrid Helix
Liu, Guang-Ning; Lin, Jian-Di; Xu, Zhong-Ning; Liu, Zhi-Fa; Guo, Guo-Cong; Huang, Jin-Shun; Crystal Growth & Design 11 (2011) 3318–; doi:10.1021/cg2005826

data_4500990
_publ_section_title
;
 Spontaneous Resolution of a New Thiogermanate Containing Chiral Binuclear
 Nickel(II) Complexes with Achiral Triethylenetetramine Ligands: A Unique
 Water-Mediated Supramolecular Hybrid Helix
;
_journal_issue                   8
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              3318
_journal_paper_doi               10.1021/cg2005826
_journal_volume                  11
_journal_year                    2011
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C18 H56 Ge4 N12 Ni2 O S10'
_chemical_formula_sum            'C18 H56 Ge4 N12 Ni2 O S10'
_chemical_formula_weight         1185.13
_chemical_melting_point          ?
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 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                   12.151(2)
_cell_length_b                   15.996(3)
_cell_length_c                   21.588(4)
_cell_measurement_reflns_used    10617
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.4971
_cell_measurement_theta_min      2.3072
_cell_volume                     4196.0(13)
_computing_cell_refinement       'CrystalClear (Rigaku Corp., 2002)'
_computing_data_collection       'CrystalClear (Rigaku Corp., 2002)'
_computing_data_reduction        'CrystalClear (Rigaku Corp., 2002)'
_computing_publication_material  'Siemens SHELXTL^TM^ 5'
_computing_structure_refinement  'Siemens SHELXTL^TM^ 5'
_computing_structure_solution    'Siemens SHELXTL^TM^ 5'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rigaku Mercury CCD'
_diffrn_measurement_method       \w
_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  0.0295
_diffrn_reflns_av_sigmaI/netI    0.0311
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            28481
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.52
_exptl_absorpt_coefficient_mu    4.241
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8413
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            pinky
_exptl_crystal_density_diffrn    1.876
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2400
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.696
_refine_diff_density_min         -0.768
_refine_diff_density_rms         0.084
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.014(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     430
_refine_ls_number_reflns         7771
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0418
_refine_ls_R_factor_gt           0.0379
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0740P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1030
_refine_ls_wR_factor_ref         0.1065
_reflns_number_gt                7200
_reflns_number_total             7771
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg2005826_si_002.cif
_cod_data_source_block           1'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not
given.

'_exptl_absorpt_correction_type' value 'Multi-scan' changed
to 'multi-scan' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        4195.9(14)
_cod_original_sg_symbol_H-M      P2(1)2(1)2(1)
_cod_database_code               4500990