Methyl 3,4-dibromo-2-(triisopropylsilyl)-1<i>H</i>-pyrrole-1-carboxylate
Martin G. Banwell; Kate E. Holden; Anthony C. Willis; Acta Crystallographica Section E 63 (2007) o3712–o3712; doi:10.1107/S1600536807037774

data_2215143
_publ_section_title
;
 Methyl
 3,4-dibromo-2-(triisopropylsilyl)-1<i>H</i>-pyrrole-1-carboxylate
;
_journal_coeditor_code           HG2268
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3712
_journal_page_last               o3712
_journal_paper_doi               10.1107/S1600536807037774
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C15 H25 Br2 N O2 Si'
_chemical_formula_moiety         'C15 H25 Br2 N O2 Si'
_chemical_formula_sum            'C15 H25 Br2 N O2 Si'
_chemical_formula_weight         439.26
_chemical_name_systematic
;
Methyl 3,4-dibromo-2-(triisopropylsilyl)-1<i>H</i>-pyrrole-1-carboxylate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method           CRYSTALS_ver_12.18
_cell_angle_alpha                90
_cell_angle_beta                 92.8487(15)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.6807(4)
_cell_length_b                   7.3800(2)
_cell_length_c                   17.4291(5)
_cell_measurement_reflns_used    92459
_cell_measurement_temperature    200
_cell_measurement_theta_max      27
_cell_measurement_theta_min      3
_cell_volume                     1886.00(9)
_computing_cell_refinement       DENZO/SCALEPACK
_computing_data_collection       'COLLECT (Nonius, 1997)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics
;
ORTEPII (Johnson, 1976) in TEXSAN (Molecular Structure Corporation,
1997)
;
_computing_publication_material  CRYSTALS
_computing_structure_refinement  'CRYSTALS (Watkin <i>et al.</i>,  2003)'
_computing_structure_solution    'SIR92 (Altomare <i>et al.</i>,  1994)'
_diffrn_ambient_temperature      200
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f and \w scans with CCD'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.059
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            41120
_diffrn_reflns_theta_full        27.516
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         3.090
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.365
_exptl_absorpt_correction_T_max  0.762
_exptl_absorpt_correction_T_min  0.447
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
[via Gaussian method (Coppens, 1970) implemented in maXus (Mackay <i>et
al.</i>,  1999)]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.547
_exptl_crystal_description       needle
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.33
_refine_diff_density_min         -0.49
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1481
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     265
_refine_ls_number_reflns         2605
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0464
_refine_ls_R_factor_gt           0.0237
_refine_ls_shift/su_max          0.002142
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial [Carruthers & Watkin (1979).
Acta Cryst. A35, 698--699; Prince (1982). Mathematical Techniques in
Crystallography and
Materials Science. New York: Springer--Verlag]
[weight] = 1/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight][1-(\dF/6\sF)^2^]^2^, A~i~ are: 2.01 -0.979 2.14 -0.341 0.473
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0324
_refine_ls_wR_factor_gt          0.0267
_refine_ls_wR_factor_ref         0.0267
_reflns_number_gt                2605
_reflns_number_total             4336
_reflns_threshold_expression     I>3\s(I)
_cod_data_source_file            hg2268.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2215143
_cod_database_fobs_code          2215143