Imposition of Chirality in a Dinuclear Triple-Stranded Helicate by Ion Pair Formation1
Robert M. Yeh; Marco Ziegler; Darren W. Johnson; Andreas J. Terpin; Kenneth N. Raymond; Inorganic Chemistry 40 (2001) 2216–2217; doi:10.1021/ic001215c

data_4319625
_publ_contact_author
;
Kenneth N. Raymond
Department of Chemistry
University of California
Berkeley, CA  94720-1460
;
_publ_contact_author_email       raymond@socrates.berkeley.edu
_publ_contact_author_fax         510-486-5283
_publ_contact_author_phone       510-642-7219
_publ_section_title
;
 Imposition of Chirality in a Dinuclear Triple-Stranded Helicate by Ion
 Pair Formation1
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2216
_journal_page_last               2217
_journal_paper_doi               10.1021/ic001215c
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C115 H121 Ga2 K N16 O18'
_chemical_formula_weight         2193.82
_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                 107.88(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.424(3)
_cell_length_b                   24.772(5)
_cell_length_c                   18.473(4)
_cell_measurement_reflns_used    10305
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.85
_cell_measurement_theta_min      1.5
_cell_volume                     6282(3)
_computing_cell_refinement
;
SMART (Siemens, 1995), SAINT (Siemens, 1995)
;
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction
;
SAINT (Siemens, 1995), XPREP (Siemens, 1995)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  '3 circle diffractometer'
_diffrn_measurement_method
;
omega scans with profile analysis
;
_diffrn_radiation_detector       'CCD area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0480
_diffrn_reflns_av_sigmaI/netI    0.0836
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            15024
_diffrn_reflns_theta_full        18.85
_diffrn_reflns_theta_max         18.85
_diffrn_reflns_theta_min         1.42
_exptl_absorpt_coefficient_mu    0.527
_exptl_absorpt_correction_T_max  0.913
_exptl_absorpt_correction_T_min  0.657
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            'reddish orange'
_exptl_crystal_density_diffrn    1.160
_exptl_crystal_density_meas      ?
_exptl_crystal_description       'fragment of needle'
_exptl_crystal_F_000             2296
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.591
_refine_diff_density_min         -0.535
_refine_diff_density_rms         0.104
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.06(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.528
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1144
_refine_ls_number_reflns         9503
_refine_ls_number_restraints     919
_refine_ls_restrained_S_all      1.467
_refine_ls_R_factor_all          0.1265
_refine_ls_R_factor_gt           0.0933
_refine_ls_shift/su_max          0.401
_refine_ls_shift/su_mean         0.012
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P]
where P=(Fo^2^+2Fc^2^)/3'
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2282
_refine_ls_wR_factor_ref         0.2426
_reflns_number_gt                7069
_reflns_number_total             9503
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic001215c.cif
_cod_data_source_block           fredsx
_cod_depositor_comments
;
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        6282(2)
_cod_original_sg_symbol_H-M      'P 21'
_cod_original_formula_sum
;
C115 H121 Ga2 K N16 O18
;
_cod_database_code               4319625