Asymmetric Twisting and Chirality Probing Properties of Quadruple-Stranded Helicates: Coordination Versatility and Chirality Response of Na+, Ca2+, and La3+ Complexes with Octadentate Cyclen Ligand
Hitomi Misaki; Hiroyuki Miyake; Satoshi Shinoda; Hiroshi Tsukube; Inorganic Chemistry 48 (2009) 11921–11928; doi:10.1021/ic901496s

data_4303839
_publ_contact_author_address
;
Department of Chemistry
Graduate School of Science
Osaka City University
3-3-138 Sugimoto, Sumiyoshi-ku, 
Osaka 558-8585, Japan
;
_publ_contact_author_name        'Prof. Hiroshi Tsukube'
_publ_section_title
;
Asymmetric Twisting and Chirality Probing Properties of Quadruple-Stranded
Helicates: Coordination Versatility and Chirality Response of Na+, Ca2+,
and La3+ Complexes with Octadentate Cyclen Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11921
_journal_page_last               11928
_journal_paper_doi               10.1021/ic901496s
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C48H50CaN8O, 2(I), 2(C2H3N), 0.25(H2O)'
_chemical_formula_sum            'C52 H56.5 Ca I2 N10 O1.25'
_chemical_formula_weight         1135.45
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                73.265(7)
_cell_angle_beta                 87.969(8)
_cell_angle_gamma                73.113(7)
_cell_formula_units_Z            2
_cell_length_a                   11.4679(14)
_cell_length_b                   13.0339(10)
_cell_length_c                   18.5389(19)
_cell_measurement_reflns_used    10790
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.4835
_cell_measurement_theta_min      4.0033
_cell_volume                     2535.7(5)
_computing_cell_refinement       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_collection       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_reduction        'CrystalClear (Rigaku Corp., 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF-99 PATTY(Beurskens, 1999)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device
;
Mercury CCD (2x2 bin mode)
;
_diffrn_measurement_method       \w
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0290
_diffrn_reflns_av_sigmaI/netI    0.0396
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            25328
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         4.00
_exptl_absorpt_coefficient_mu    1.390
_exptl_absorpt_correction_T_max  0.8735
_exptl_absorpt_correction_T_min  0.6806
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Jacobson, 1998)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.487
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1149
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.539
_refine_diff_density_min         -0.760
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.140
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     601
_refine_ls_number_reflns         11342
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.140
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0428
_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^)+(0.0058P)^2^+6.8011P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0723
_refine_ls_wR_factor_ref         0.0757
_reflns_number_gt                9968
_reflns_number_total             11342
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901496s_si_002_2.cif
_cod_data_source_block           '[Ca(1)(H2O)]I2(CH3CN)2(H2O)0.25'
_cod_depositor_comments
;
The following automatic conversions were performed:
'_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_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        2535.7(4)
_cod_original_formula_sum        'C52 H56.50 Ca I2 N10 O1.25'
_cod_database_code               4303839