Gold-catalyzed (4 + 2)-annulations between α-alkyl alkenylgold carbenes and benzisoxazoles with reactive alkyl groups.
Mokar, Bhanudas Dattatray; Jadhav, Prakash D.; Pandit, Y. B.; Liu, Rai-Shung; Chemical science 9 (2018) 4488–4492; doi:10.1039/c8sc00986d

data_1549280
_publ_section_title
;
 Gold-catalyzed (4 + 2)-annulations between \a-alkyl alkenylgold carbenes
 and benzisoxazoles with reactive alkyl groups.
;
_journal_issue                   19
_journal_name_full               'Chemical science'
_journal_page_first              4488
_journal_page_last               4492
_journal_paper_doi               10.1039/c8sc00986d
_journal_volume                  9
_journal_year                    2018
_chemical_formula_sum            'C21.5 H19.5 Cl1.5 N O3'
_chemical_formula_weight         393.05
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2018-01-24 deposited with the CCDC.
2018-04-23 downloaded from the CCDC.
;
_cell_angle_alpha                84.071(19)
_cell_angle_beta                 88.539(15)
_cell_angle_gamma                84.074(13)
_cell_formula_units_Z            4
_cell_length_a                   11.282(7)
_cell_length_b                   11.457(7)
_cell_length_c                   14.934(9)
_cell_measurement_reflns_used    6877
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.0475
_cell_measurement_theta_min      2.2687
_cell_volume                     1910(2)
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.959
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0495
_diffrn_reflns_av_unetI/netI     0.0585
_diffrn_reflns_Laue_measured_fraction_full 0.959
_diffrn_reflns_Laue_measured_fraction_max 0.960
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_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6443
_diffrn_reflns_point_group_measured_fraction_full 0.959
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_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         1.371
_exptl_absorpt_coefficient_mu    0.292
_exptl_absorpt_correction_T_max  0.9484
_exptl_absorpt_correction_T_min  0.8556
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/4 (Bruker AXS Inc.)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.367
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Tabullar
_exptl_crystal_F_000             820
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.04
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_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     494
_refine_ls_number_reflns         6443
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0704
_refine_ls_R_factor_gt           0.0451
_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^)+(0.0476P)^2^+0.1940P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0929
_refine_ls_wR_factor_ref         0.1031
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4896
_reflns_number_total             6443
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc00986d2.cif
_cod_data_source_block           TWIN5
_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 4973 2017-02-22 13:04:09Z antanas 

2019-02-18
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel

 Adding full bibliography for 1549278--1549281.cif.
;
_cod_original_cell_volume        1909(2)
_cod_original_formula_sum        'C43 H39 Cl3 N2 O6'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     786.11
_cod_database_code               1549280
_shelxl_version_number           2014/6
_shelx_res_checksum              45978