A solution-phase route to a tetraethynylated (cyclobutadiene)cyclopentadienylcobalt complex with a para-(1,3,2,4)-substitution patternElectronic supplementary information (ESI) available: experimental, including details of preparation and spectroscopic characterization of all new compounds. See http://www.rsc.org/suppdata/cc/b1/b109848a/
Laskoski, Matthew; Morton, Jason G. M.; Smith, Mark D.; Bunz, Uwe H. F.; Chemical Communications  (2001) 2590–; doi:10.1039/b109848a

data_7114829
_publ_section_title
;
 A solution-phase route to a tetraethynylated
 (cyclobutadiene)cyclopentadienylcobalt complex with a
 para-(1,3,2,4)-substitution patternElectronic supplementary information
 (ESI) available: experimental, including details of preparation and
 spectroscopic characterization of all new compounds. See
 http://www.rsc.org/suppdata/cc/b1/b109848a/
;
_journal_issue                   24
_journal_name_full               'Chemical Communications'
_journal_page_first              2590
_journal_paper_doi               10.1039/b109848a
_journal_year                    2001
_chemical_formula_sum            'C37.25 H33.5 Cl0.5 Co'
_chemical_formula_weight         557.80
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.163(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   23.132(2)
_cell_length_b                   18.932(2)
_cell_length_c                   29.492(4)
_cell_measurement_reflns_used    4526
_cell_measurement_temperature    190(2)
_cell_measurement_theta_max      22.701
_cell_measurement_theta_min      2.267
_cell_volume                     12626(2)
_computing_cell_refinement       'SAINT+ NT V6.02a (Bruker, 1998)'
_computing_data_collection       'SMART NT V5.624 (Bruker, 2000)'
_computing_data_reduction        'SAINT+ NT V6.02a'
_computing_molecular_graphics    'SHELXTL V5.1 (Sheldrick, 1997)'
_computing_publication_material  'SHELXTL V5.1'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      190(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker SMART APEX CCD diffractometer'
_diffrn_measurement_method       'omega 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  0.0989
_diffrn_reflns_av_sigmaI/netI    0.1338
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            22647
_diffrn_reflns_theta_full        22.80
_diffrn_reflns_theta_max         22.80
_diffrn_reflns_theta_min         1.40
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    0.608
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.174
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       bar
_exptl_crystal_F_000             4680
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.464
_refine_diff_density_min         -0.261
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     748
_refine_ls_number_reflns         8515
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.1344
_refine_ls_R_factor_gt           0.0699
_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 
[0.00000+1.00000exp(1.00(sin\q/\l)^2^)]/ 
[\s^2^(Fo^2^)+0.0000+0.0000*P+(0.0568P)^2^+0.0000sin\q/\l] 
where P = 0.33333Fo^2^ + 0.66667Fc^2^ 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1379
_refine_ls_wR_factor_ref         0.1616
_reflns_number_gt                4430
_reflns_number_total             8515
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b109848a.txt
_cod_data_source_block           mlsublm
_cod_original_cell_volume        12626(3)
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C37.25 H33.50 Cl0.50 Co'
_cod_database_code               7114829