Synthesis, structure, and reactivity of (triphenylarsoranylidene)methylcyclohepta-2,4,6-trienone derivatives: reactions with heterocumulenes and an activated acetylene
Mitsumoto, Yuhki; Nitta, Makoto; Journal of the Chemical Society, Perkin Transactions 1  (2002) 2268–; doi:10.1039/b205612g

data_7205037
_publ_section_title
;
 Synthesis, structure, and reactivity of
 (triphenylarsoranylidene)methylcyclohepta-2,4,6-trienone derivatives:
 reactions with heterocumulenes and an activated acetylene
;
_journal_issue                   20
_journal_name_full
'Journal of the Chemical Society, Perkin Transactions 1'
_journal_page_first              2268
_journal_paper_doi               10.1039/b205612g
_journal_year                    2002
_chemical_compound_source        'Local laboratory'
_chemical_formula_moiety         'C29 H25 As O3 '
_chemical_formula_sum            'C29 H25 As O3'
_chemical_formula_weight         496.438
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           maXus
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.021(6)
_cell_length_b                   8.864(5)
_cell_length_c                   15.780(6)
_cell_measurement_temperature    250
_cell_volume                     2380.8(18)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_orient_matrix_type       X=UH
_diffrn_orient_matrix_UB_11      0.06177
_diffrn_orient_matrix_UB_12      0.01078
_diffrn_orient_matrix_UB_13      -0.01438
_diffrn_orient_matrix_UB_21      -0.01189
_diffrn_orient_matrix_UB_22      0.05770
_diffrn_orient_matrix_UB_23      -0.00218
_diffrn_orient_matrix_UB_31      0.00773
_diffrn_orient_matrix_UB_32      0.00251
_diffrn_orient_matrix_UB_33      0.11188
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           ' CuK\a'
_diffrn_radiation_wavelength_id  all
_diffrn_reflns_av_R_equivalents  0.068
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            9091
_diffrn_reflns_theta_full        70.02
_diffrn_reflns_theta_max         70.02
_exptl_absorpt_coefficient_mu    2.155
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.385
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Cube
_refine_diff_density_max         0.490
_refine_diff_density_min         -0.662
_refine_diff_density_rms         0.067
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.05(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.581
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     297
_refine_ls_number_reflns         4449
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.581
_refine_ls_R_factor_all          0.0482
_refine_ls_R_factor_gt           0.0482
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+ (0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1520
_refine_ls_wR_factor_ref         0.1522
_reflns_number_gt                4441
_reflns_number_total             4449
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b205612g.txt
_cod_data_source_block           global
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        2381.(2)
_cod_original_sg_symbol_H-M      'P n a 21      '
_cod_original_formula_sum        'C29 H25 As O3 '
_cod_database_code               7205037