Photochromic Atropisomer Generation and Conformation Determination in a Ruthenium Bis(bipyridine) Phosphonite γ-Cyclodextrin System
Dusan Hesek; Guy A. Hembury; Michael G. B. Drew; Victor V. Borovkov; Yoshihisa Inoue; Journal of the American Chemical Society 123 (2001) 12232–12237; doi:10.1021/ja0116167

data_4115837
_publ_section_title
;
 Photochromic Atropisomer Generation and Conformation Determination in a
 Ruthenium Bis(bipyridine) Phosphonite \g-Cyclodextrin System
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12232
_journal_page_last               12237
_journal_paper_doi               10.1021/ja0116167
_journal_volume                  123
_journal_year                    2001
_chemical_formula_sum            'C28 H27 Cl F6 N4 O2 P2 Ru'
_chemical_formula_weight         764.10
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 103.61(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.700(3)
_cell_length_b                   13.608(2)
_cell_length_c                   18.681(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      14.9
_cell_measurement_theta_min      14.6
_cell_volume                     3137.8(9)
_computing_cell_refinement       'Rigaku/AFC Diffractometer Control'
_computing_data_collection       'Rigaku/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_molecular_graphics    PLATON(Spek,1994)
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_computing_structure_solution    'DIRDIF92 (PATTY)'
_diffrn_ambient_temperature      296.2
_diffrn_measured_fraction_theta_full 0.958
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device_type  'scintillation counter'
_diffrn_measurement_method       \w-2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0847
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            7211
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         2.66
_diffrn_standards_decay_%        0.265
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.759
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.779
_exptl_absorpt_correction_type   'w scans (North,Phillips and Mathews, 1968)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.626
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1544
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.714
_refine_diff_density_min         -0.835
_refine_diff_density_rms         0.095
_refine_ls_extinction_coef       0.0000(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.975
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     400
_refine_ls_number_reflns         7211
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.975
_refine_ls_R_factor_all          0.1259
_refine_ls_R_factor_gt           0.0456
_refine_ls_shift/su_max          0.665
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0766P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1202
_refine_ls_wR_factor_ref         0.1495
_reflns_number_gt                4029
_reflns_number_total             7211
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0116167.cif
_cod_data_source_block           cis-[Ru(bpy)2(PhP(OMe)2)(Cl)]PF6(2)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0766P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0766P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3137.9(8)
_cod_original_formula_sum        'C28 H27 Cl F6 N4 O2 P2 Ru1'
_cod_database_code               4115837