Synthesis, Structure, and Kinetics and Stereochemistry of Base-Catalyzed Hydrolysis of meso- and rac-[Co2(tmpdtne)Cl2]4+, Bis(pentaamine) Complexes Devoid of Deprotonatable NH Centers
Jackson, W. Gregory; Dickie, Alistair J.; McKeon, Josephine A.; Spiccia, Leone; Brudenell, Suzanne J.; Hockless, David C. R.; Willis, Anthony C.; Inorganic Chemistry 44 (2005) 401–409; doi:10.1021/ic0400888

data_4308358
_publ_section_title
;
 Synthesis, Structure, and Kinetics and Stereochemistry of Base-Catalyzed
 Hydrolysis of meso- and rac-[Co2(tmpdtne)Cl2]4+, Bis(pentaamine) Complexes
 Devoid of Deprotonatable NH Centers
;
_journal_coden_ASTM              INOCAJ
_journal_issue                   2
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              401
_journal_page_last               409
_journal_paper_doi               10.1021/ic0400888
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety         'C38 H56 Co2 N10 O2 4+, 4(Cl O4 -), 3(H2 O)'
_chemical_formula_sum            'C38 H62 Cl4 Co2 N10 O21'
_chemical_formula_weight         1254.64
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_audit_creation_date             2002-05-15
_audit_creation_method           'by teXsan v1.8'
_audit_update_record
;
1997-06-05 - Report on C38 H62 Cl4 Co2 N10 O21
               by David C.R. Hockless
               for W. Greg Jackson, ADFA
2002-05-16 - acw  compiles cif
2002-05-16 - passes checkcif tests with warnings
;
_cell_angle_alpha                90
_cell_angle_beta                 94.98(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.331(3)
_cell_length_b                   23.353(5)
_cell_length_c                   16.478(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      26.4
_cell_measurement_theta_min      20.3
_cell_volume                     5111(2)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan (MSC, 1992-1997)'
_computing_publication_material  'teXsan (MSC, 1992-1997)'
_computing_structure_refinement  'teXsan (MSC, 1992-1997)'
_computing_structure_solution
;
SIR92 (Altomare, et. al. 1994)
;
_diffrn_ambient_temperature      296.2
_diffrn_measurement_device_type  'Rigaku AFC6R'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      -0.00330
_diffrn_orient_matrix_UB_12      -0.01134
_diffrn_orient_matrix_UB_13      -0.05869
_diffrn_orient_matrix_UB_21      -0.04034
_diffrn_orient_matrix_UB_22      0.03512
_diffrn_orient_matrix_UB_23      -0.01504
_diffrn_orient_matrix_UB_31      0.06349
_diffrn_orient_matrix_UB_32      0.02172
_diffrn_orient_matrix_UB_33      -0.00633
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.12853
_diffrn_reflns_av_sigmaI/netI    0.310
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            8189
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         60.04
_diffrn_reflns_theta_min         1.89
_diffrn_standards_decay_%        -1.54
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    7.779
_exptl_absorpt_correction_T_max  .537
_exptl_absorpt_correction_T_min  .282
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
\y scans (North,Phillips & Matthews, 1968)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.631
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             2600.00
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.61
_refine_diff_density_min         -0.66
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.500
_refine_ls_goodness_of_fit_ref   2.096
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     331
_refine_ls_number_reflns         1630
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.3506
_refine_ls_R_factor_gt           0.0901
_refine_ls_shift/su_max          0.0160
_refine_ls_shift/su_mean         0.0020
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00016|Fo|^2^]'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.1270
_refine_ls_wR_factor_ref         0.0764
_reflns_number_gt                1630
_reflns_number_total             7586
_reflns_threshold_expression     I>3.00\s(I)
_cod_data_source_file            ic0400888.cif
_cod_data_source_block           hockWGJ5
_cod_original_sg_symbol_H-M      'P 21/a '
_cod_original_formula_sum        'C38 H62 Cl4 Co2 N10 O21 '
_cod_database_code               4308358