An Efficient Synthesis of Novel Fused Cycloheptatrienes through Mn(II)-Mediated Formal Intermolecular [2 + 2 + 2 + 1] Cycloaddition.
Shu, Wen-Ming; Ma, Jun-Rui; Yang, Yan; Wu, An-Xin; Organic letters 16 (2014) 1286–1289; doi:10.1021/ol500202q

data_1513824
_publ_section_title
;
 An Efficient Synthesis of Novel Fused Cycloheptatrienes through
 Mn(II)-Mediated Formal Intermolecular [2 + 2 + 2 + 1] Cycloaddition.
;
_journal_issue                   5
_journal_name_full               'Organic letters'
_journal_page_first              1286
_journal_page_last               1289
_journal_paper_doi               10.1021/ol500202q
_journal_volume                  16
_journal_year                    2014
_chemical_formula_sum            'C42 H25 Cl O9'
_chemical_formula_weight         709.07
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_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                102.481(2)
_cell_angle_beta                 108.708(2)
_cell_angle_gamma                101.479(2)
_cell_formula_units_Z            2
_cell_length_a                   10.9599(15)
_cell_length_b                   12.1631(17)
_cell_length_c                   14.371(2)
_cell_measurement_reflns_used    5263
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      31.27
_cell_measurement_theta_min      2.30
_cell_volume                     1695.4(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
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_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.57
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.173
_exptl_absorpt_correction_T_max  0.9829
_exptl_absorpt_correction_T_min  0.9795
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.389
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             732
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
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_refine_diff_density_max         0.447
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_refine_ls_extinction_method     none
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_refine_ls_number_parameters     471
_refine_ls_number_reflns         6223
_refine_ls_number_restraints     0
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_refine_ls_R_factor_all          0.0630
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_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0937P)^2^+0.5852P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1497
_refine_ls_wR_factor_ref         0.1654
_reflns_number_gt                4923
_reflns_number_total             6223
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol500202q_si_001.cif
_cod_data_source_block           e:\130522a\work\mo_130522a_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        1695.5(4)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1513824