Crystal engineering in the <i>gem</i>-alkynol family: the key role of water in the structure of 2,3,5,6-tetrabromo-<i>trans</i>-1,4-diethynyl-cyclohexa-2,5-diene-1,4-diol dihydrate determined by X-ray and neutron diffraction at 150K
Bilton, Clair; Howard, Judith A. K.; Madhavi, N. N. L.; Desiraju, Gautam R.; Allen, Frank H.; Wilson, Chick C.; Acta Crystallographica Section B 57 (2001) 560–566; doi:10.1107/S0108768101008412

data_2103685
_publ_section_title
;
 Crystal engineering in the <i>gem</i>-alkynol family: the key role of
 water in the structure of
 2,3,5,6-tetrabromo-<i>trans</i>-1,4-diethynyl-cyclohexa-2,5-diene-1,4-diol
 dihydrate determined by X-ray and neutron diffraction at 150K
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              560
_journal_page_last               566
_journal_paper_doi               10.1107/S0108768101008412
_journal_volume                  57
_journal_year                    2001
_chemical_formula_sum            'C10 H8 Br4 O4'
_chemical_formula_weight         511.80
_space_group_IT_number           138
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4ac 2ac'
_symmetry_space_group_name_H-M   'P 42/n c m :2'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.6551(18)
_cell_length_b                   12.6551(18)
_cell_length_c                   8.7340(17)
_cell_measurement_reflns_used    999
_cell_measurement_temperature    150
_cell_measurement_theta_max      23.25
_cell_measurement_theta_min      2.28
_cell_volume                     1398.8(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean 'not relevant'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Brucker SMART CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .0302
_diffrn_reflns_av_sigmaI/netI    .0120
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            6046
_diffrn_reflns_theta_full        23.25
_diffrn_reflns_theta_max         23.25
_diffrn_reflns_theta_min         2.28
_exptl_absorpt_coefficient_mu    11.510
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  .644
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'multi-scan, using SADABS'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.430
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             960
_exptl_crystal_size_max          .4
_exptl_crystal_size_mid          .3
_exptl_crystal_size_min          .3
_refine_diff_density_max         .441
_refine_diff_density_min         -.298
_refine_ls_extinction_coef       .0039(3)
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.224
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     58
_refine_ls_number_reflns         539
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.224
_refine_ls_R_factor_all          .0219
_refine_ls_R_factor_gt           .0201
_refine_ls_shift/su_max          .000
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0231P)^2^+2.4727P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .0532
_reflns_number_gt                501
_reflns_number_total             539
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            bm0041.cif
_cod_data_source_block           nmbrX
_cod_original_sg_symbol_H-M      P4(2)/ncm
_cod_database_code               2103685
_cod_database_fobs_code          2103685