The synthesis of substituted phosphathiahelicenes via regioselective bromination of a preformed helical scaffold: a new approach to modular ligands for enantioselective gold-catalysis.
Aillard, Paul; Dova, Davide; Magné, Valentin; Retailleau, Pascal; Cauteruccio, Silvia; Licandro, Emanuela; Voituriez, Arnaud; Marinetti, Angela; Chemical communications (Cambridge, England) 52 (2016) 10984–10987; doi:10.1039/c6cc04765c

data_7124808
_publ_section_title
;
 The synthesis of substituted phosphathiahelicenes via regioselective
 bromination of a preformed helical scaffold: a new approach to modular
 ligands for enantioselective gold-catalysis.
;
_journal_issue                   73
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              10984
_journal_page_last               10987
_journal_paper_doi               10.1039/c6cc04765c
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety         'C60 H62 Au Cl P S3'
_chemical_formula_sum            'C60 H62 Au Cl P S3'
_chemical_formula_weight         1142.66
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-05-07 deposited with the CCDC.
2016-08-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.590(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.8334(14)
_cell_length_b                   21.319(3)
_cell_length_c                   12.7266(18)
_cell_measurement_reflns_used    568
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      51.0
_cell_measurement_theta_min      6.8
_cell_volume                     2655.3(7)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.0 r8 (Rigaku, 2011)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r8 (Rigaku, 2011)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.0 r8 (Rigaku, 2011)
;
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXD-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'Curved IP Rapid2'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device
;
Crystal Goniometer
;
_diffrn_measurement_device_type
;
Rigaku RAXIS conversion
;
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support Fiber
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.1240
_diffrn_reflns_av_unetI/netI     0.2752
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13030
_diffrn_reflns_point_group_measured_fraction_full 0.753
_diffrn_reflns_point_group_measured_fraction_max 0.753
_diffrn_reflns_theta_full        66.574
_diffrn_reflns_theta_max         66.574
_diffrn_reflns_theta_min         3.490
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    7.334
_exptl_absorpt_correction_T_max  0.60
_exptl_absorpt_correction_T_min  0.20
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Fs_process (Rigaku)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.429
_exptl_crystal_description       'elongated platelet'
_exptl_crystal_F_000             1162
_exptl_crystal_size_max          0.370
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.137
_refine_diff_density_min         -1.244
_refine_diff_density_rms         0.120
_refine_ls_abs_structure_details
;
 Flack x determined using 661 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.00(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.958
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     601
_refine_ls_number_reflns         7062
_refine_ls_number_restraints     578
_refine_ls_restrained_S_all      0.925
_refine_ls_R_factor_all          0.2175
_refine_ls_R_factor_gt           0.0837
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0881P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1848
_refine_ls_wR_factor_ref         0.2576
_reflns_Friedel_coverage         0.504
_reflns_Friedel_fraction_full    0.520
_reflns_Friedel_fraction_max     0.520
_reflns_number_gt                2610
_reflns_number_total             7065
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc04765c2.cif
_cod_data_source_block           helphos-S-Ph-AuCl
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7124808
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              13783