Brine-Stabilized 2,2,2-Trifluorodiazoethane and Its Application in the Synthesis of CF3-Substituted Cyclopropane α-Amino Acids.
Zhu, Chuan-Le; Yang, Li-Jun; Li, Shen; Zheng, Yan; Ma, Jun-An; Organic letters 17 (2015) 3442–3445; doi:10.1021/acs.orglett.5b01450

data_1520726
_publ_section_title
;
 Brine-Stabilized 2,2,2-Trifluorodiazoethane and Its Application in the
 Synthesis of CF3-Substituted Cyclopropane \a-Amino Acids.
;
_journal_issue                   14
_journal_name_full               'Organic letters'
_journal_page_first              3442
_journal_page_last               3445
_journal_paper_doi               10.1021/acs.orglett.5b01450
_journal_volume                  17
_journal_year                    2015
_chemical_formula_sum            'C44 H42 F6 N6 O7 S2'
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_space_group_IT_number           61
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_symmetry_space_group_name_Hall  '-P 2ac 2ab'
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_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   21.512(10)
_cell_length_b                   10.424(5)
_cell_length_c                   40.881(18)
_cell_measurement_temperature    294(2)
_cell_volume                     9167(7)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2085
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_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            82447
_diffrn_reflns_theta_full        26.45
_diffrn_reflns_theta_max         26.45
_diffrn_reflns_theta_min         3.01
_exptl_absorpt_coefficient_mu    0.196
_exptl_absorpt_correction_T_max  0.9883
_exptl_absorpt_correction_T_min  0.9544
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.369
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3920
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.519
_refine_diff_density_min         -0.331
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     589
_refine_ls_number_reflns         9415
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.2430
_refine_ls_R_factor_gt           0.1095
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0922P)^2^+6.2872P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2310
_refine_ls_wR_factor_ref         0.2997
_reflns_number_gt                3547
_reflns_number_total             9415
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol5b01450_si_002.cif
_cod_data_source_block           130826a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/usr/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.

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

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 1520726--1520727.cif.
;
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               1520726