Structural Studies on the Stepwise Chelating Processes of Bidentate 2-(Aminomethyl)pyridine and Tridentate Bis(2-pyridylmethyl)amine toward an Acetate-Bridged Dirhodium(II) Center
Takashi Yoshimura; Keisuke Umakoshi; Yoichi Sasaki; Inorganic Chemistry 42 (2003) 7106–7115; doi:10.1021/ic030093w

data_4312363
_publ_contact_author_address
;
        Division of Chemistry
    Graduate School of Science
    Hokkaido University
    Kita-ku, Sapporo 060-0810
    Japan
;
_publ_contact_author_email       ' ysasaki@sci.hokudai.ac.jp '
_publ_contact_author_fax         ' +81-11-706-3817 '
_publ_contact_author_name        ' Prof. Yoichi Sasaki'
_publ_contact_author_phone       ' +81-11-706-3447 '
_publ_section_title
;
 Structural Studies on the Stepwise Chelating Processes of Bidentate
 2-(Aminomethyl)pyridine and Tridentate Bis(2-pyridylmethyl)amine toward
 an Acetate-Bridged Dirhodium(II) Center
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7106
_journal_page_last               7115
_journal_paper_doi               10.1021/ic030093w
_journal_volume                  42
_journal_year                    2003
_chemical_formula_moiety         'C34 H32 F12 N6 O4 P2 Rh2 '
_chemical_formula_sum            'C69 H68 F24 N12 O9 P4 Rh4'
_chemical_formula_weight         1100.43
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                106.60(1)
_cell_angle_beta                 91.77(1)
_cell_angle_gamma                87.07(1)
_cell_formula_units_Z            4
_cell_length_a                   15.553(2)
_cell_length_b                   21.871(3)
_cell_length_c                   13.338(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      15.0
_cell_measurement_theta_min      11.1
_cell_volume                     4341.6(11)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_molecular_graphics    ORTEP
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      296.2
_diffrn_measurement_device       'Rigaku AFC5R'
_diffrn_measurement_method       '\w/2\q scans'
_diffrn_orient_matrix_UB_11      -0.01051
_diffrn_orient_matrix_UB_12      0.00454
_diffrn_orient_matrix_UB_13      0.07542
_diffrn_orient_matrix_UB_21      -0.02890
_diffrn_orient_matrix_UB_22      0.04295
_diffrn_orient_matrix_UB_23      0.00758
_diffrn_orient_matrix_UB_31      -0.05657
_diffrn_orient_matrix_UB_32      -0.02038
_diffrn_orient_matrix_UB_33      -0.01940
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.023
_diffrn_reflns_av_sigmaI/netI    0.081
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            20658
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.56
_diffrn_standards_decay_%        -0.19
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.929
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.761
_exptl_absorpt_correction_type   '\y scans(North,Phillips & Mathews,1968)'
_exptl_crystal_colour            'orange red'
_exptl_crystal_density_diffrn    1.683
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2188.00
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.76
_refine_diff_density_min         -0.68
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   5.107
_refine_ls_hydrogen_treatment    'H atoms riding with U(H) = 1.2Ueq(C)'
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     1089
_refine_ls_number_reflns         10344
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0699
_refine_ls_shift/esd_max         0.3370
_refine_ls_shift/esd_mean        0.0180
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.000012|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.0809
_reflns_number_observed          10344
_reflns_number_total             19922
_reflns_observed_criterion       I>2.5sigma(I)
_cod_data_source_file            ic030093w_5.cif
_cod_data_source_block           '[Rh2(CH3COO)2(bpy)2(py)2](PF6)2.(0.5)CH3OH'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'w = 1/[\s^2^(Fo) +
0.000012|Fo|^2^]' was changed to 'calc'. New tag
'_refine_ls_weighting_details' was created. The value of the new tag
was set to 'w = 1/[\s^2^(Fo) + 0.000012|Fo|^2^]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        4341(1)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C69 H68 F24 N12 O9 P4 Rh4 '
_cod_database_code               4312363