Intermolecular Three-Component Arylsilylation of Alkynes under Palladium/Copper Cooperative Catalysis.
Shintani, Ryo; Kurata, Hiroki; Nozaki, Kyoko; The Journal of organic chemistry 81 (2016) 3065–3069; doi:10.1021/acs.joc.6b00587

data_4036812
_publ_section_title
;
 Intermolecular Three-Component Arylsilylation of Alkynes under
 Palladium/Copper Cooperative Catalysis.
;
_journal_issue                   8
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              3065
_journal_page_last               3069
_journal_paper_doi               10.1021/acs.joc.6b00587
_journal_volume                  81
_journal_year                    2016
_chemical_formula_sum            'C24 H17 Br'
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_space_group_crystal_system      monoclinic
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_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 104.854(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.793(6)
_cell_length_b                   5.631(3)
_cell_length_c                   13.738(6)
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_cell_measurement_temperature    93
_cell_measurement_theta_max      31.0
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_cell_volume                     881.8(8)
_computing_cell_refinement
;
Rigaku CrystalClear-SM Expert 2.0 r3
;
_computing_data_collection
;
Rigaku CrystalClear-SM Expert 2.0 r3
;
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;
Rigaku CrystalClear-SM Expert 2.0 r3
;
_computing_molecular_graphics    'Yadokari-XG 2009 (Wakita Nemoto et al., 2009)'
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_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      93
_diffrn_detector_area_resol_mean 28.5714
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_diffrn_measured_fraction_theta_max 0.899
_diffrn_measurement_device_type  'Rigaku Saturn724 CCD'
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_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_source         'rotating-anode X-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0400
_diffrn_reflns_av_unetI/netI     0.0642
_diffrn_reflns_Laue_measured_fraction_full 0.997
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_diffrn_reflns_theta_max         31.272
_diffrn_reflns_theta_min         2.637
_diffrn_source                   'Rotating Anode'
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_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communicatio'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.451
_exptl_crystal_description       Block
_exptl_crystal_F_000             392
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.368
_refine_diff_density_min         -0.734
_refine_diff_density_rms         0.086
_refine_ls_abs_structure_details
;
 Flack x determined using 1306 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.070(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         4609
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0501
_refine_ls_R_factor_gt           0.0438
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0439P)^2^+0.2516P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0951
_refine_ls_wR_factor_ref         0.1014
_reflns_Friedel_coverage         0.636
_reflns_Friedel_fraction_full    0.895
_reflns_Friedel_fraction_max     0.686
_reflns_number_gt                4201
_reflns_number_total             4609
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo6b00587_si_003.cif
_cod_data_source_block           ydkr
_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/ACS/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               4036812
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.593
_shelx_estimated_absorpt_t_max   0.933
_shelx_res_checksum              74018
_shelx_hkl_checksum              52895