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_1551336
_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         489.276
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.2835(2)
_cell_length_b                   12.3657(4)
_cell_length_c                   24.4205(10)
_cell_measurement_reflns_used    33991
_cell_measurement_temperature    223
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      2.425
_cell_volume                     2199.45(13)
_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, 1997)'
_computing_structure_solution    'SIR97(Altomare et al., J. Appl. Cryst.,1999)'
_diffrn_ambient_temperature      223
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device       KappaCCD
_diffrn_measurement_method       CCD
_diffrn_orient_matrix_type       X=UH
_diffrn_orient_matrix_UB_11      0.02607
_diffrn_orient_matrix_UB_12      0.13297
_diffrn_orient_matrix_UB_13      0.02211
_diffrn_orient_matrix_UB_21      -0.05204
_diffrn_orient_matrix_UB_22      0.01995
_diffrn_orient_matrix_UB_23      -0.05860
_diffrn_orient_matrix_UB_31      -0.03036
_diffrn_orient_matrix_UB_32      0.00139
_diffrn_orient_matrix_UB_33      0.02744
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           ' MoK\a'
_diffrn_radiation_wavelength_id  all
_diffrn_reflns_av_R_equivalents  0.093
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            15682
_diffrn_reflns_theta_full        24.98
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         4.10
_exptl_absorpt_coefficient_mu    1.920
_exptl_absorpt_correction_T_max  0.964
_exptl_absorpt_correction_T_min  0.732
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Gaussian integration (Coppens, 1970)
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.478
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1000.0
_exptl_crystal_size_max          .36
_exptl_crystal_size_mid          .09
_exptl_crystal_size_min          .02
_refine_diff_density_max         0.738
_refine_diff_density_min         -0.559
_refine_diff_density_rms         0.064
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.011(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     275
_refine_ls_number_reflns         3827
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0756
_refine_ls_R_factor_gt           0.0559
_refine_ls_shift/su_max          0.049
_refine_ls_shift/su_mean         0.001
_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          0.1501
_refine_ls_wR_factor_ref         0.1645
_reflns_number_gt                3043
_reflns_number_total             3827
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            nchem.1575-s4.cif
_cod_data_source_block           p1_ccdc848429
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Orthorhombic' was changed
to 'orthorhombic' 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      'P 21 21 21    '
_cod_original_formula_sum        'C19 H21 Br O10 '
_cod_database_code               1551336