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_1507458
_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(C7 H8)'
_chemical_formula_sum            'C37.5 H31 Co'
_chemical_formula_weight         540.59
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_date             'Fri Sep 21 15:48:07 2001'
_audit_creation_method           'by teXsan plus manual editing'
_cell_angle_alpha                111.494(2)
_cell_angle_beta                 95.570(2)
_cell_angle_gamma                100.867(2)
_cell_formula_units_Z            2
_cell_length_a                   7.0791(7)
_cell_length_b                   13.176(1)
_cell_length_c                   15.734(2)
_cell_measurement_reflns_used    2211
_cell_measurement_temperature    149.2
_cell_measurement_theta_max      22.5
_cell_measurement_theta_min      1.8
_cell_volume                     1318.7(2)
_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 0.9289
_diffrn_measured_fraction_theta_max 0.9289
_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       8
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            4179
_diffrn_reflns_theta_full        24.73
_diffrn_reflns_theta_max         24.73
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.677
_exptl_absorpt_correction_T_max  0.990
_exptl_absorpt_correction_T_min  0.880
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sortav Blessing, 1995'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.360
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.47
_refine_diff_density_min         -0.65
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.593
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     346
_refine_ls_number_reflns         2988
_refine_ls_R_factor_gt           0.0532
_refine_ls_shift/su_max          0.0003
_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         0.0649
_reflns_number_gt                2988
_reflns_number_total             4179
_reflns_threshold_expression     F^2^>3.0\s(F^2^)
_cod_data_source_file            ol025956o_s2.cif
_cod_data_source_block           pid371
_cod_depositor_comments
;
 Marking atom 'C100' as a dummy atom.

 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      P-1
_cod_original_formula_sum        'C37.50 H31 Co'
_cod_database_code               1507458