Synthesis, crystal structure and properties of thiaheterohelicenes containing phenolic hydroxy functions
Kitahara, Yoshinori; Tanaka, Kazuhiko; Chemical Communications  (2002) 932–; doi:10.1039/b110514k

data_7114526
_publ_section_title
;
 Synthesis, crystal structure and properties of thiaheterohelicenes
 containing phenolic hydroxy functions
;
_journal_issue                   9
_journal_name_full               'Chemical Communications'
_journal_page_first              932
_journal_paper_doi               10.1039/b110514k
_journal_year                    2002
_chemical_formula_moiety         'C28 H18 O2 S2 '
_chemical_formula_sum            'C28 H18 O2 S2'
_chemical_formula_weight         450.57
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_audit_creation_date             'Wed Oct 25 10:24:29 2000'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.719(6)
_cell_length_b                   17.730(4)
_cell_length_c                   9.974(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298.2
_cell_measurement_theta_max      15.0
_cell_measurement_theta_min      14.2
_cell_volume                     2072.4(14)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_diffrn_ambient_temperature      298.2
_diffrn_measurement_device       'Rigaku AFC5R'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      0.06044
_diffrn_orient_matrix_UB_12      0.03912
_diffrn_orient_matrix_UB_13      0.01315
_diffrn_orient_matrix_UB_21      0.05788
_diffrn_orient_matrix_UB_22      -0.04062
_diffrn_orient_matrix_UB_23      0.01461
_diffrn_orient_matrix_UB_31      0.01669
_diffrn_orient_matrix_UB_32      -0.00081
_diffrn_orient_matrix_UB_33      -0.09832
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.000
_diffrn_reflns_av_sigmaI/netI    0.071
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            2720
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         2.68
_diffrn_standards_decay_%        1.25
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.282
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.975
_exptl_absorpt_correction_type   '\y scans(North,Phillips & Mathews,1968)'
_exptl_crystal_colour            pail
_exptl_crystal_density_diffrn    1.444
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             936.00
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.300
_refine_diff_density_max         0.17
_refine_diff_density_min         -0.24
_refine_ls_extinction_coef       0.004(3)
_refine_ls_extinction_method     'Zachariasen(1967) type 2 Gaussian isotropic'
_refine_ls_goodness_of_fit_obs   1.229
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     290
_refine_ls_number_reflns         1759
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0528
_refine_ls_shift/esd_max         0.0000
_refine_ls_shift/esd_mean        0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00265|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.0770
_reflns_number_observed          1759
_reflns_number_total             2720
_reflns_observed_criterion       >2.0sigma(I)
_cod_data_source_file            b110514k.txt
_cod_data_source_block           crystal_(P)-4_or_(M)-4;_dimethoxyhelicene
_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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'w = 1/[\s^2^(Fo) +
0.00265|Fo|^2^]' 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) + 0.00265|Fo|^2^]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2072(1)
_cod_original_sg_symbol_H-M      'P 21 21 21   '
_cod_original_formula_sum        'C28 H18 O2 S2 '
_cod_database_code               7114526