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_4312359
_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         'C38 H32 Cl2 N6 O8 Rh2 '
_chemical_formula_sum            'C38 H32 Cl2 N6 O8 Rh2'
_chemical_formula_weight         977.42
_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                97.98(1)
_cell_angle_beta                 112.78(1)
_cell_angle_gamma                72.63(1)
_cell_formula_units_Z            1
_cell_length_a                   9.652(2)
_cell_length_b                   14.198(2)
_cell_length_c                   8.013(1)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      14.9
_cell_measurement_theta_min      12.5
_cell_volume                     965.9(3)
_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    SAPI91
_diffrn_ambient_temperature      296.2
_diffrn_measurement_device       'Rigaku AFC5R'
_diffrn_measurement_method       '\w/2\q scans'
_diffrn_orient_matrix_UB_11      0.03424
_diffrn_orient_matrix_UB_12      0.05893
_diffrn_orient_matrix_UB_13      -0.00596
_diffrn_orient_matrix_UB_21      -0.08718
_diffrn_orient_matrix_UB_22      0.01680
_diffrn_orient_matrix_UB_23      -0.11936
_diffrn_orient_matrix_UB_31      -0.06950
_diffrn_orient_matrix_UB_32      0.04116
_diffrn_orient_matrix_UB_33      0.06365
_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  0.022
_diffrn_reflns_av_sigmaI/netI    0.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4761
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         2.5
_diffrn_standards_decay_%        0.44
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.038
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.680
_exptl_crystal_density_meas      ?
_exptl_crystal_description       rhombic
_exptl_crystal_F_000             490.00
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.81
_refine_diff_density_min         -0.88
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   4.041
_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     252
_refine_ls_number_reflns         3810
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0499
_refine_ls_shift/esd_max         0.0010
_refine_ls_shift/esd_mean        0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.000004|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.0586
_reflns_number_observed          3810
_reflns_number_total             4442
_reflns_observed_criterion       I>2.0sigma(I)
_cod_data_source_file            ic030093w_1.cif
_cod_data_source_block           '[Rh2(OAc)4(Cl-tpy)2]'
_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) +
0.000004|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) + 0.000004|Fo|^2^]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        966.0(3)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C38 H32 Cl2 N6 O8 Rh2 '
_cod_database_code               4312359