Csp-Csp(3) Bond Formation via Iron(III)-Promoted Hydroalkynylation of Unactivated Alkenes.
Shen, Yangyong; Huang, Bo; Zheng, Jing; Lin, Chen; Liu, Yu; Cui, Sunliang; Organic letters 19 (2017) 1744–1747; doi:10.1021/acs.orglett.7b00499

data_1545659
_publ_section_title
;
 Csp-Csp(3) Bond Formation via Iron(III)-Promoted Hydroalkynylation of
 Unactivated Alkenes.
;
_journal_issue                   7
_journal_name_full               'Organic letters'
_journal_page_first              1744
_journal_page_last               1747
_journal_paper_doi               10.1021/acs.orglett.7b00499
_journal_volume                  19
_journal_year                    2017
_chemical_formula_sum            'C28 H32 O'
_chemical_formula_weight         384.54
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_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
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_atom_sites_solution_primary     direct
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_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.243(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.429(6)
_cell_length_b                   8.033(4)
_cell_length_c                   13.269(7)
_cell_measurement_reflns_used    2165
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      22.35
_cell_measurement_theta_min      2.38
_cell_volume                     1107.0(10)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'SHELXTL(Sheldrick, 2008)'
_computing_publication_material  'WINGX (Farrugia,1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare,1999)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX2 CCD area-detector diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
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_diffrn_reflns_limit_h_max       12
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_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7614
_diffrn_reflns_theta_full        27.24
_diffrn_reflns_theta_max         27.24
_diffrn_reflns_theta_min         1.54
_exptl_absorpt_coefficient_mu    0.068
_exptl_absorpt_correction_T_max  0.9839
_exptl_absorpt_correction_T_min  0.9774
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.154
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             416
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.089
_refine_diff_density_min         -0.116
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_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.4(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
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_refine_ls_matrix_type           full
_refine_ls_number_parameters     266
_refine_ls_number_reflns         4773
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0720
_refine_ls_R_factor_gt           0.0430
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0379P)^2^+0.0383P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0873
_refine_ls_wR_factor_ref         0.1011
_reflns_number_gt                3281
_reflns_number_total             4773
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol7b00499_si_003.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 1545659.cif.
;
_cod_original_sg_symbol_H-M      'P21   '
_cod_database_code               1545659