Computational and synthetic studies with tetravinylethylenes.
Lindeboom, Erik J.; Willis, Anthony C.; Paddon-Row, Michael N; Sherburn, Michael S.; The Journal of organic chemistry 79 (2014) 11496–11507; doi:10.1021/jo5021294

data_4030230
_publ_section_title
;
 Computational and synthetic studies with tetravinylethylenes.
;
_journal_issue                   23
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              11496
_journal_page_last               11507
_journal_paper_doi               10.1021/jo5021294
_journal_volume                  79
_journal_year                    2014
_chemical_absolute_configuration unk
_chemical_compound_source        local
_chemical_formula_moiety         'C22 H44 Si4'
_chemical_formula_sum            'C22 H44 Si4'
_chemical_formula_weight         420.93
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             12-10-29
_audit_creation_method           CRYSTALS_ver_14.11
_audit_update_record
; 
2012-10-230 - Report on C26 H28 Br N O2 
             by Anthony C. Willis 
             for Erik J. Lindeboom and Mick Sherburn 
2012-10-230 - passes checkcif tests with minor warnings 
;
_cell_angle_alpha                90
_cell_angle_beta                 113.385(2)
_cell_angle_gamma                90
_cell_formula_units_Z            6
_cell_length_a                   18.4241(7)
_cell_length_b                   12.7737(5)
_cell_length_c                   20.9954(5)
_cell_measurement_reflns_used    89322
_cell_measurement_temperature    200
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2.6
_cell_volume                     4535.3(3)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics
; 
ORTEP-II (Johnson 1976) in teXsan (MSC, 1992-1997)
;
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
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_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      200
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
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_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            65729
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_diffrn_reflns_theta_min         2.648
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.201
_exptl_absorpt_correction_T_max  0.981
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_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
via Gaussian method (Coppens, 1970) implemented in maXus (2000)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    0.925
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.280
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_refine_diff_density_max         0.79
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_refine_ls_abs_structure_details
;
The space group is polar but,
in the absence of significant anomalous scattering, 
the Friedel pairs have been merged
and the absolute structure has not been determined. 
The molecule has no chiral centres.
;
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9832
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     703
_refine_ls_number_reflns         8338
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1332
_refine_ls_R_factor_gt           0.0914
_refine_ls_shift/su_max          0.0353180
_refine_ls_shift/su_mean         0.0065928
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[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-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 196. 326. 189. 71.4 13.8 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2986
_refine_ls_wR_factor_gt          0.2390
_refine_ls_wR_factor_ref         0.2986
_reflns_limit_h_max              20
_reflns_limit_h_min              -21
_reflns_limit_k_max              15
_reflns_limit_k_min              0
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                5163
_reflns_number_total             8341
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   5.13
_oxford_diffrn_Wilson_scale      13.33
_oxford_refine_ls_r_factor_ref   0.1332
_oxford_refine_ls_scale          0.3482(10)
_oxford_reflns_number_all        8338
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title '10291148 she1233'
_cod_data_source_file            jo5021294_si_003.cif
_cod_data_source_block           she1233
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/home/saulius/struct/COD-crude-data--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 2935 2014-11-11 08:27:57Z andrius 

 Adding full bibliography for 4030223--4030230.cif.
;
_cod_original_sg_symbol_H-M      'P 1 21 1 '
_cod_database_code               4030230
_iucr_refine_instruction_details_constraints
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END                                                                             
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_iucr_refine_instruction_details_restraints
;
NO 
END                                                                             
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