Progress toward the Total Synthesis of N-Methylwelwitindolinone B Isothiocyanate.
Cleary, Leah; Pitzen, Jennifer; Brailsford, John A.; Shea, Kenneth J.; Organic letters 16 (2014) 4460–; doi:10.1021/ol5020043

data_1517385
_publ_section_title
;
 Progress toward the Total Synthesis of N-Methylwelwitindolinone B
 Isothiocyanate.
;
_journal_issue                   17
_journal_name_full               'Organic letters'
_journal_page_first              4460
_journal_paper_doi               10.1021/ol5020043
_journal_volume                  16
_journal_year                    2014
_chemical_formula_sum            'C21 H22 Cl N O5'
_chemical_formula_weight         403.84
_space_group_crystal_system      monoclinic
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_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
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_atom_sites_solution_secondary   difmap
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_cell_angle_beta                 98.3270(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.0367(6)
_cell_length_b                   9.0626(5)
_cell_length_c                   19.1081(10)
_cell_measurement_reflns_used    5758
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      28.52
_cell_measurement_theta_min      2.28
_cell_volume                     1891.07(18)
_computing_cell_refinement       'Bruker SAINT 7.68a, 2009'
_computing_data_collection       'Bruker APEX2 2010.3-0, 2010'
_computing_data_reduction        'Bruker SAINT 7.68a, 2009'
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_computing_structure_solution    'Bruker SHELXTL 2008/4'
_diffrn_ambient_temperature      93(2)
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_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
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_diffrn_reflns_limit_l_min       -25
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_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
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_diffrn_source                   'fine-focus sealed tube'
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_exptl_absorpt_correction_T_max  1.0000
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_exptl_absorpt_correction_type   numerical
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_exptl_crystal_colour            colorless
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_exptl_crystal_density_meas      ?
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_refine_ls_R_factor_all          0.0430
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_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0426P)^2^+0.9200P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0842
_refine_ls_wR_factor_ref         0.0889
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3829
_reflns_number_total             4475
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol5020043_si_003.cif
_cod_data_source_block           kjs71
_cod_depositor_comments
;Adding full bibliography for 1517385--1517386.cif.

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               1517385
_shelx_estimated_absorpt_t_min   0.926
_shelx_estimated_absorpt_t_max   0.972
_shelxl_version_number           2013-3
_shelx_res_checksum              56387
_shelx_hkl_checksum              94436