Crystal structures of (μ~2~-η^2^,η^2^-4-hydroxybut-2-yn-1-yl 2-bromo-2-methylpropanoate-κ^4^<i>C</i>^2^,<i>C</i>^3^:<i>C</i>^2^,<i>C</i>^3^)bis[tricarbonylcobalt(II)](<i>Co{—</i>Co}) and [μ~2~-η^2^,η^2^-but-2-yne-1,4-diyl bis(2-bromo-2-methylpropanoate)-κ^4^<i>C</i>^2^,<i>C</i>^3^:<i>C</i>^2^,<i>C</i>^3^]bis[tricarbonylcobalt(II)](<i>Co{—</i>Co})
McAdam, C. John; Moratti, Stephen C.; Robinson, Brian H.; Simpson, Jim; Stanley, Roderick G.; Acta Crystallographica Section E 70 (2014) 9–13; doi:10.1107/S1600536814009659

data_2239739
_publ_section_title
;
 Crystal structures of (\m~2~-\h^2^,\h^2^-4-hydroxybut-2-yn-1-yl
 2-bromo-2-methylpropanoate-\k^4^<i>C</i>^2^,<i>C</i>^3^:<i>C</i>^2^,<i>C</i>^3^)bis[tricarbonylcobalt(II)](<i>Co{---</i>Co})
 and [\m~2~-\h^2^,\h^2^-but-2-yne-1,4-diyl
 bis(2-bromo-2-methylpropanoate)-\k^4^<i>C</i>^2^,<i>C</i>^3^:<i>C</i>^2^,<i>C</i>^3^]bis[tricarbonylcobalt(II)](<i>Co{---</i>Co})
;
_journal_coeditor_code           HB0001
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              9
_journal_page_last               13
_journal_paper_doi               10.1107/S1600536814009659
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          '[Co2 (C8 H11 Br O3) (C O)6]'
_chemical_formula_moiety         'C14 H11 Br Co2 O9'
_chemical_formula_sum            'C14 H11 Br Co2 O9'
_chemical_formula_weight         521.00
_chemical_name_systematic
'[\m~2~-\h^2^,\h^2^-4-Hydroxybut-2-yn-1-yl 2-bromo-2-methylpropanoate-\k^4^<i>C</i>^2^,<i>C</i>^3^:<i>C</i>^2^,<i>C</i>^3^]bis[tricarbonylcobalt(II)](<i>Co</i>---<i>Co</i>)'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                78.583(6)
_cell_angle_beta                 85.239(6)
_cell_angle_gamma                76.342(6)
_cell_formula_units_Z            2
_cell_length_a                   7.3887(8)
_cell_length_b                   11.1147(12)
_cell_length_c                   11.7274(13)
_cell_measurement_reflns_used    3089
_cell_measurement_temperature    91(2)
_cell_measurement_theta_max      51.239
_cell_measurement_theta_min      4.721
_cell_volume                     916.67(18)
_computing_cell_refinement       'APEX2 and SAINT (Bruker, 2011)'
_computing_data_collection       'APEX2 (Bruker, 2011)'
_computing_data_reduction        'SAINT (Bruker, 2011)'
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>, 2008)
;
_computing_publication_material
;
SHELXL2013 (Sheldrick, 2008), enCIFer (Allen <i>et al.</i>,
2004), PLATON
(Spek, 2009) and publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2013 (Sheldrick, 2008) and <i>TITAN2000</i> (Hunter & Simpson,
1999)
;
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      91(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0547
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11686
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.523
_diffrn_reflns_theta_min         3.287
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.032
_exptl_absorpt_correction_T_max  0.8554
_exptl_absorpt_correction_T_min  0.3023
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2011)'
_exptl_crystal_colour            orange-red
_exptl_crystal_density_diffrn    1.888
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular fragment'
_exptl_crystal_F_000             512
_exptl_crystal_size_max          0.390
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.833
_refine_diff_density_min         -0.727
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     238
_refine_ls_number_reflns         3713
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0541
_refine_ls_R_factor_gt           0.0375
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0486P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0900
_refine_ls_wR_factor_ref         0.0973
_reflns_number_gt                2966
_reflns_number_total             3713
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb0001sup1.cif
_cod_data_source_block           1
_cod_database_code               2239739
_cod_database_fobs_code          2239739
_shelx_estimated_absorpt_t_min   0.302
_shelx_estimated_absorpt_t_max   0.855
_shelx_hkl_checksum              72944
_shelx_res_checksum              22043