Gold-catalyzed [4+3] and [4+4]-annulation reactions of t-butyl propiolate derivatives with epoxides and oxetanes for the construction of 1,4-dioxepane and 1,5-dioxocane cores
Rajkumar Lalji Sahani; Rai-Shung Liu; Chem.Commun. 52 (2016) 7482–; doi:

data_7119174
_publ_section_title
;
 Gold-catalyzed [4+3] and [4+4]-annulation reactions of t-butyl propiolate
 derivatives with epoxides and oxetanes for the construction of
 1,4-dioxepane and 1,5-dioxocane cores
;
_journal_name_full               Chem.Commun.
_journal_page_first              7482
_journal_volume                  52
_journal_year                    2016
_chemical_formula_sum            'C18 H16 O4'
_chemical_formula_weight         296.30
_space_group_crystal_system      monoclinic
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_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2016-02-24 deposited with the CCDC.
2016-05-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.262(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.8910(9)
_cell_length_b                   16.2219(12)
_cell_length_c                   15.2941(11)
_cell_measurement_reflns_used    2346
_cell_measurement_temperature    296(2)
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_cell_measurement_theta_min      2.4573
_cell_volume                     2945.4(4)
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
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_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
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_computing_publication_material  SHELXTL
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_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
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_diffrn_reflns_number            25025
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.387
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_exptl_absorpt_coefficient_mu    0.094
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_exptl_absorpt_process_details   'SADABS V2014/4 (Bruker AXS Inc.)'
_exptl_crystal_colour            Yellow
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_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Lump
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_refine_ls_R_factor_all          0.0986
_refine_ls_R_factor_gt           0.0489
_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^)+(0.0903P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1296
_refine_ls_wR_factor_ref         0.1720
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3433
_reflns_number_total             6020
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc02124g2.cif
_cod_data_source_block           151129_0m
_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 4624 2016-04-14 12:54:50Z antanas 

2017-03-03
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum        'C36 H32 O8'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     592.61
_cod_database_code               7119174
_shelxl_version_number           2014/6
_shelx_res_checksum              26471