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_4312360
_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_sum            'C30 H38 F6 N6 O7.5 P Rh2'
_chemical_formula_weight         953.44
_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                103.98(1)
_cell_angle_beta                 101.025(10)
_cell_angle_gamma                74.808(10)
_cell_formula_units_Z            2
_cell_length_a                   13.569(2)
_cell_length_b                   16.015(2)
_cell_length_c                   9.056(1)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    293.2
_cell_measurement_theta_max      12.1
_cell_measurement_theta_min      10.1
_cell_volume                     1825.6(4)
_computing_cell_refinement       'Rigaku/AFC Diffractometer Control'
_computing_data_collection       'Rigaku/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_diffrn_ambient_temperature      293.2
_diffrn_measurement_device       'Rigaku AFC7S'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      0.05000
_diffrn_orient_matrix_UB_12      0.03891
_diffrn_orient_matrix_UB_13      0.04113
_diffrn_orient_matrix_UB_21      0.05834
_diffrn_orient_matrix_UB_22      -0.05335
_diffrn_orient_matrix_UB_23      -0.00293
_diffrn_orient_matrix_UB_31      0.00630
_diffrn_orient_matrix_UB_32      0.00208
_diffrn_orient_matrix_UB_33      -0.10722
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.030
_diffrn_reflns_av_sigmaI/netI    0.112
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            8760
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.57
_diffrn_standards_decay_%        -1.25
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.031
_exptl_absorpt_correction_T_max  0.998
_exptl_absorpt_correction_T_min  0.947
_exptl_absorpt_correction_type   '\y scans(North,Phillips & Mathews,1968)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.734
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             958.00
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.94
_refine_diff_density_min         -0.47
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   1.059
_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     468
_refine_ls_number_reflns         4242
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0525
_refine_ls_shift/esd_max         0.1780
_refine_ls_shift/esd_mean        0.0120
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00672|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.0982
_reflns_number_observed          4242
_reflns_number_total             8404
_reflns_observed_criterion       >2.0sigma(I)
_cod_data_source_file            ic030093w_2.cif
_cod_data_source_block           '[Rh2(m-CH3COO)2(h-CH3COO)(bpa)2]PF6.(1.5)H2O'
_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) +
0.00672|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) + 0.00672|Fo|^2^]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1825.7(4)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C30 H38 F6 N6 O7.50 P Rh2 '
_cod_database_code               4312360