Thermal reactivities of isostructural d10 metalloenediynes: metal-dependent Bergman cyclization
Schmitt, Elbert W.; Huffman, John C.; Zaleski, Jeffrey M.; Chemical Communications  (2001) 167–; doi:10.1039/b008337m

data_7114741
_publ_section_title
;
 Thermal reactivities of isostructural d10 metalloenediynes:
 metal-dependent Bergman cyclization
;
_journal_issue                   2
_journal_name_full               'Chemical Communications'
_journal_page_first              167
_journal_paper_doi               10.1039/b008337m
_journal_year                    2001
_chemical_formula_sum            'C68 H54 Ag F6 O3 P5'
_chemical_formula_weight         1295.9
_space_group_IT_number           26
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P -2 -2b'
_symmetry_space_group_name_H-M   'P b 21 m'
_audit_creation_method
'minor manual editing of SDT2CIF v. 1.2 BETA  output'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.4950(4)
_cell_length_b                   20.2486(7)
_cell_length_c                   28.7007(9)
_cell_measurement_reflns_used    5268
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.40
_cell_measurement_theta_min      2.48
_cell_volume                     6680.3(4)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        'SAINT (Bruker, 1999), XTEL (local package)'
_computing_molecular_graphics    'XTEL, local package'
_computing_publication_material  'XTEL, local package'
_computing_structure_refinement  'XTEL, local package'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      113(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 44.52
_diffrn_detector_type            'Bruker SMART 6000'
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_diffrn_measurement_details
'   0.30 degree frames measured for  10.13 seconds each'
_diffrn_measurement_device       'three-circle goniometer with fixed chi'
_diffrn_measurement_device_type  'Bruker Platform goniometer'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.063
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            53276
_diffrn_reflns_theta_full        27.5509
_diffrn_reflns_theta_max         27.5509
_diffrn_reflns_theta_min         2.03713
_diffrn_standards_decay_%        0.0
_diffrn_standards_interval_time  215
_diffrn_standards_number         5269
_exptl_absorpt_coefficient_mu    0.4802
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.734492
_exptl_absorpt_correction_type   semi-empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.289
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'square plate'
_exptl_crystal_F_000             2648
_exptl_crystal_size_max          .40
_exptl_crystal_size_mid          .40
_exptl_crystal_size_min          .15
_refine_diff_density_max         1.47
_refine_diff_density_min         -0.67
_refine_ls_abs_structure_details none
_refine_ls_extinction_coef       -0.00000011(2)
_refine_ls_extinction_expression
;                                                                               
Larson, A. C. (1967).  Acta Cryst. 23, p. 664.  Eq. (3)                         
;
_refine_ls_extinction_method     Zachariasen
_refine_ls_goodness_of_fit_ref   1.4965
_refine_ls_matrix_type           full
_refine_ls_number_parameters     778
_refine_ls_number_reflns         4819
_refine_ls_R_factor_gt           0.0574
_refine_ls_shift/su_max          0.0734
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     w^-1^=\s^2^(F)+(.07F)^2^
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0737
_reflns_number_gt                4819
_reflns_number_total             8056
_reflns_threshold_expression     'Fo^2^> 2.33\s(Fo^2^)'
_cod_data_source_file            b008337m.txt
_cod_data_source_block           MSC00091
_cod_original_formula_sum        'C68 H54 Ag1 F6 O3 P5'
_cod_database_code               7114741