Cobalt-Mediated Synthesis of Angular [4]Phenylene: Structural Characterization of a Metallacyclopentadiene(Alkyne) Intermediate and Its Thermal and Photochemical Conversion
Dosa, Peter I.; Whitener, Glenn D.; Vollhardt, K. Peter C.; Bond, Andrew D.; Teat, Simon J.; Organic Letters 4 (2002) 2075–; doi:10.1021/ol025956o

data_1507459
_publ_section_title
;
 Cobalt-Mediated Synthesis of Angular [4]Phenylene: Structural
 Characterization of a Metallacyclopentadiene(Alkyne) Intermediate and Its
 Thermal and Photochemical Conversion
;
_journal_issue                   12
_journal_name_full               'Organic Letters'
_journal_page_first              2075
_journal_paper_doi               10.1021/ol025956o
_journal_volume                  4
_journal_year                    2002
_chemical_formula_moiety         'C34 H27 Co, 0.5(C4 H8 O)'
_chemical_formula_sum            'C36 H31 Co O0.5'
_chemical_formula_weight         530.57
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_audit_creation_date             'Fri Sep 21 15:48:07 2001'
_audit_creation_method           'by teXsan plus manual editing'
_cell_angle_alpha                90
_cell_angle_beta                 96.501(1)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.4895(8)
_cell_length_b                   9.0045(5)
_cell_length_c                   40.411(2)
_cell_measurement_reflns_used    3247
_cell_measurement_temperature    138.2
_cell_measurement_theta_max      22.5
_cell_measurement_theta_min      1.5
_cell_volume                     5238.5(5)
_computing_cell_refinement       'Bruker SAINT v5.04'
_computing_data_collection       'Bruker SMART v5.0'
_computing_data_reduction        'Bruker SAINT v5.04'
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_computing_structure_solution    SIR97
_diffrn_measured_fraction_theta_full 0.8962
_diffrn_measured_fraction_theta_max 0.8962
_diffrn_measurement_device_type  'SMART CCD'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.047
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            4739
_diffrn_reflns_theta_full        25.64
_diffrn_reflns_theta_max         25.64
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.681
_exptl_absorpt_correction_T_max  0.934
_exptl_absorpt_correction_T_min  0.589
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.55
_refine_diff_density_min         -0.59
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.316
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     333
_refine_ls_number_reflns         2605
_refine_ls_R_factor_gt           0.0394
_refine_ls_shift/su_max          0.0005
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00022|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0396
_reflns_number_gt                2605
_reflns_number_total             4440
_reflns_threshold_expression     F^2^>3.0\s(F^2^)
_cod_data_source_file            ol025956o_s2.cif
_cod_data_source_block           PID385
_cod_depositor_comments
;
 Marking atoms 'C100' and 'C101' as dummy atoms.

 Antanas Vaitkus,
 2017-02-19

 Changing the values of data items related to the _atom_site_label data item
 (e. g. _geom_bond_atom_site_label_*) to match the _atom_site_label values.

 Antanas Vaitkus,
 2017-01-06
;
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C36 H31 Co O0.50'
_cod_database_code               1507459