An Organic Intermolecular Dehydrogenative Annulation Reaction.
Maiti, Saikat; Achar, Tapas Kumar; Mal, Prasenjit; Organic letters 19 (2017) 2006–2009; doi:10.1021/acs.orglett.7b00562

data_1545745
_publ_section_title
;
 An Organic Intermolecular Dehydrogenative Annulation Reaction.
;
_journal_issue                   8
_journal_name_full               'Organic letters'
_journal_page_first              2006
_journal_page_last               2009
_journal_paper_doi               10.1021/acs.orglett.7b00562
_journal_volume                  19
_journal_year                    2017
_chemical_formula_sum            'C20 H19 N O2 S'
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_symmetry_space_group_name_H-M   'P c a 21'
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_atom_sites_solution_secondary   difmap
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_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.6695(7)
_cell_length_b                   5.5971(3)
_cell_length_c                   39.2584(19)
_cell_measurement_reflns_used    4231
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      20.55
_cell_measurement_theta_min      3.67
_cell_volume                     3443.1(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_limit_h_max       20
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_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            51449
_diffrn_reflns_theta_full        28.05
_diffrn_reflns_theta_max         28.05
_diffrn_reflns_theta_min         2.65
_exptl_absorpt_coefficient_mu    0.199
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6622
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   Sadabs
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.302
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.416
_refine_diff_density_min         -0.274
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_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.2(3)
_refine_ls_extinction_coef       0.005(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     440
_refine_ls_number_reflns         8242
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      3.054
_refine_ls_R_factor_all          0.1255
_refine_ls_R_factor_gt           0.0680
_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^)+(0.1301P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1815
_refine_ls_wR_factor_ref         0.2245
_reflns_number_gt                4597
_reflns_number_total             8242
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol7b00562_si_003.cif
_cod_data_source_block           try
_cod_depositor_comments
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The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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 1545745--1545747.cif.

2019-01-19
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
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_cod_original_sg_symbol_H-M      'Pca2(1) '
_cod_original_formula_sum        'C40 H38 N2 O4 S2'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     674.84
_cod_database_code               1545745