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_7114740
_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            'C70 H52 Cl4 Cu F6 P5'
_chemical_formula_weight         1367.4
_space_group_IT_number           57
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2c 2b'
_symmetry_space_group_name_H-M   'P b c 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                   11.5309(4)
_cell_length_b                   20.2376(7)
_cell_length_c                   28.5051(11)
_cell_measurement_reflns_used    4098
_cell_measurement_temperature    135(2)
_cell_measurement_theta_max      26.56
_cell_measurement_theta_min      2.47
_cell_volume                     6651.9(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      135(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  15.14 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       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            45044
_diffrn_reflns_theta_full        27.5206
_diffrn_reflns_theta_max         27.5206
_diffrn_reflns_theta_min         2.15465
_diffrn_standards_decay_%        0.0
_diffrn_standards_interval_time  321
_diffrn_standards_number         4099
_exptl_absorpt_coefficient_mu    0.6663
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.897536
_exptl_absorpt_correction_type   semi-empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.365
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2792
_exptl_crystal_size_max          .18
_exptl_crystal_size_mid          .32
_exptl_crystal_size_min          .4
_refine_diff_density_max         1.15
_refine_diff_density_min         -1.37
_refine_ls_abs_structure_details none
_refine_ls_extinction_coef       -0.00000006(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   1.2380
_refine_ls_matrix_type           full
_refine_ls_number_parameters     421
_refine_ls_number_reflns         3589
_refine_ls_R_factor_gt           0.0495
_refine_ls_shift/su_max          0.0524
_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         0.0610
_reflns_number_gt                3589
_reflns_number_total             6846
_reflns_threshold_expression     'Fo^2^> 2.33\s(Fo^2^)'
_cod_data_source_file            b008337m.txt
_cod_data_source_block           MSC00096
_cod_original_formula_sum        'C70 H52 Cl4 Cu1 F6 P5'
_cod_database_code               7114740