Polypyrazolylmethane complexes of ruthenium
Field, Leslie D.; Messerle, Barbara A.; Soler, Linnea; Buys, Irmi E.; Hambley, Trevor W.; Journal of the Chemical Society, Dalton Transactions  (2001) 1959–1965; doi:10.1039/b103939n

data_7010804
_publ_section_title
;
 Polypyrazolylmethane complexes of ruthenium
;
_journal_coden_ASTM              JCSDAA
_journal_issue                   13
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1959
_journal_page_last               1965
_journal_paper_doi               10.1039/b103939n
_journal_year                    2001
_chemical_formula_sum            'C56 H54 Cl2 N6 O2.2 P2.33 Ru'
_chemical_formula_weight         1090.43
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-P 3*'
_space_group_name_H-M_alt        'R -3 :R'
_cell_angle_alpha                90.73(2)
_cell_angle_beta                 90.73(2)
_cell_angle_gamma                90.73(2)
_cell_formula_units_Z            6
_cell_length_a                   20.022(4)
_cell_length_b                   20.022(4)
_cell_length_c                   20.022(4)
_cell_measurement_reflns_used    5084
_cell_measurement_temperature    273.2
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.0
_cell_volume                     8024(3)
_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
;
SHELXS86 (Sheldrick, 1985)
;
_diffrn_ambient_temperature      273.2
_diffrn_measurement_device_type  CAD-4
_diffrn_orient_matrix_UB_11      0.02336
_diffrn_orient_matrix_UB_12      -0.04067
_diffrn_orient_matrix_UB_13      0.01626
_diffrn_orient_matrix_UB_21      0.01473
_diffrn_orient_matrix_UB_22      -0.01019
_diffrn_orient_matrix_UB_23      -0.04657
_diffrn_orient_matrix_UB_31      0.04167
_diffrn_orient_matrix_UB_32      0.02731
_diffrn_orient_matrix_UB_33      0.00823
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.05512
_diffrn_reflns_av_sigmaI/netI    0.080
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            10977
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.01
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.510
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.354
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             3375.30
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.49
_refine_diff_density_min         -0.42
_refine_ls_extinction_coef       0.000000062(9)
_refine_ls_extinction_expression 'equ(3) Acta Cryst.(1968) A24, p213.'
_refine_ls_extinction_method     'Zachariasen (1967)'
_refine_ls_goodness_of_fit_all   1.861
_refine_ls_goodness_of_fit_ref   2.172
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    12
_refine_ls_number_parameters     606
_refine_ls_number_reflns         4785
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0873
_refine_ls_R_factor_gt           0.0476
_refine_ls_shift/su_max          0.1606
_refine_ls_shift/su_mean         0.0077
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo)]'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.0544
_refine_ls_wR_factor_ref         0.0514
_reflns_number_gt                4785
_reflns_number_total             7262
_reflns_threshold_expression     I>2.50\s(I)
_cod_data_source_file            b103939n.txt
_cod_data_source_block           E_LDF42
_cod_depositor_comments
;
 Correcting the space group by changing it from 'R -3 :H' to 'R -3 :R' after
 consulting the original publication.

 Antanas Vaitkus,
 2018-01-28
;
_cod_original_cell_volume        8024.5(8)
_cod_original_sg_symbol_H-M      'R -3       '
_cod_original_formula_sum        'C56 H54 Cl2 N6 O2.20 P2.33 Ru '
_cod_database_code               7010804