A multistep single-crystal-to-single-crystal bromodiacetylene dimerization
Tobias N. Hoheisel; Stephen Schrettl; Roman Marty; Tanya K. Todorova; Clemence Corminboeuf; Andrzej Sienkiewicz; Rosario Scopelliti; W. Bernd Schweizer; Holger Frauenrath; Nature Chemistry 5 (2013) 327–334; doi:10.1038/nchem.1575

data_1551335
_publ_section_title
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 A multistep single-crystal-to-single-crystal bromodiacetylene
 dimerization
;
_journal_name_full               'Nature Chemistry'
_journal_page_first              327
_journal_page_last               334
_journal_paper_doi               10.1038/nchem.1575
_journal_volume                  5
_journal_year                    2013
_chemical_compound_source        'MAT ETH Zurich'
_chemical_formula_moiety         'C19 H21 Br O10 '
_chemical_formula_sum            'C19 H21 Br O10'
_chemical_formula_weight         489.271
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 117.232(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   28.5038(3)
_cell_length_b                   6.6628(6)
_cell_length_c                   13.4137(7)
_cell_measurement_reflns_used    8492
_cell_measurement_temperature    173
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      2.425
_cell_volume                     2265.1(2)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       KappaCCD
_computing_data_reduction
'Denzo and Scalepak (Otwinowski & Minor, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device       KappaCCD
_diffrn_measurement_method       CCD
_diffrn_orient_matrix_type       X=UH
_diffrn_orient_matrix_UB_11      -0.07150
_diffrn_orient_matrix_UB_12      -0.01260
_diffrn_orient_matrix_UB_13      0.13715
_diffrn_orient_matrix_UB_21      -0.04419
_diffrn_orient_matrix_UB_22      -0.06886
_diffrn_orient_matrix_UB_23      -0.01833
_diffrn_orient_matrix_UB_31      0.02571
_diffrn_orient_matrix_UB_32      -0.06840
_diffrn_orient_matrix_UB_33      0.02979
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           ' MoK\a'
_diffrn_radiation_wavelength_id  all
_diffrn_reflns_av_R_equivalents  0.0659
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9770
_diffrn_reflns_theta_full        25.04
_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_min         3.76
_exptl_absorpt_coefficient_mu    1.86
_exptl_absorpt_correction_T_max  0.81344
_exptl_absorpt_correction_T_min  0.49811
_exptl_absorpt_correction_type   gaussian
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          .3
_exptl_crystal_size_mid          .2
_exptl_crystal_size_min          .1
_refine_diff_density_max         0.482
_refine_diff_density_min         -0.292
_refine_diff_density_rms         0.061
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.367
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     310
_refine_ls_number_reflns         3923
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.382
_refine_ls_R_factor_all          0.1130
_refine_ls_R_factor_gt           0.0808
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+ (0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2071
_refine_ls_wR_factor_ref         0.2282
_reflns_number_gt                2686
_reflns_number_total             3923
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            nchem.1575-s3.cif
_cod_data_source_block           sc030309
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Gaussian' was
changed to 'gaussian' in accordance with the built-in table derived
from the CIF Core dictionary named 'cif_core.dic' version 2.4.5 last
updated on 2014-11-21.

data item '_symmetry_cell_setting' value 'Monoclinic' was changed to
'monoclinic' in accordance with the built-in table derived from the
CIF Core dictionary named 'cif_core.dic' version 2.4.5 last updated
on 2014-11-21.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      'C 2           '
_cod_original_formula_sum        'C19 H21 Br O10 '
_cod_database_code               1551335