Geminal Dehydrogenation of Ether and Amine C(sp^3^)H~2~ Groups by Electron-Rich Ru(II) and Os
Ferrando-Miguel, German; Coalter, III, Joseph N.; Gérard, Hélène; Huffman, John C.; Eisenstein, Odile; Caulton, Kenneth G.; New Journal of Chemistry 26 (2002) 687–700; doi:10.1039/b200168n

data_5000291
_publ_contact_author_address
;
Department of Chemistry
Indiana University
Bloomington
47405-4001
UNITED STATES OF AMERICA
;
_publ_contact_author_email       CAULTON@INDIANA.EDU
_publ_contact_author_name        'Dr. Caulton, K. G.'
_publ_section_title
;
 Geminal Dehydrogenation of Ether and Amine C(sp^3^)H~2~ Groups by
 Electron-Rich Ru(II) and Os
;
_journal_coden_ASTM              NJCHE5
_journal_issue                   6
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              687
_journal_page_last               700
_journal_paper_doi               10.1039/b200168n
_journal_volume                  26
_journal_year                    2002
_chemical_formula_moiety         ?
_chemical_formula_sum            'C22 H50 Cl N P2 Ru'
_chemical_formula_weight         527.116
_space_group_IT_number           36
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'C 2c -2'
_symmetry_space_group_name_H-M   'C m c 21'
_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                   21.4753(7)
_cell_length_b                   8.8416(3)
_cell_length_c                   13.4685(4)
_cell_measurement_reflns_used    4733
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      29.96
_cell_measurement_theta_min      2.49
_cell_volume                     2557.35(14)
_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      153(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   5.15 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  0.049
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            12198
_diffrn_reflns_theta_full        30.0205
_diffrn_reflns_theta_max         30.0205
_diffrn_reflns_theta_min         2.49118
_diffrn_standards_decay_%        0.0
_diffrn_standards_interval_time  109
_diffrn_standards_number         4734
_exptl_absorpt_coefficient_mu    0.8512
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.819023
_exptl_absorpt_correction_type   semi-empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.369
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'triangular plate'
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          .3
_exptl_crystal_size_mid          .3
_exptl_crystal_size_min          .1
_refine_diff_density_max         0.7
_refine_diff_density_min         -0.34
_refine_ls_abs_structure_details none
_refine_ls_abs_structure_Flack   ?
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.8602
_refine_ls_hydrogen_treatment    ?
_refine_ls_matrix_type           full
_refine_ls_number_parameters     119
_refine_ls_number_reflns         2495
_refine_ls_R_factor_gt           0.0276
_refine_ls_shift/su_max          0.0002
_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         0.0307
_reflns_number_gt                2495
_reflns_number_total             3094
_reflns_threshold_expression     'Fo^2^> 2.33\s(Fo^2^)'
_cod_original_formula_sum        'C22 H50 Cl1 N1 P2 Ru1'
_cod_database_code               5000291