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_7010803
_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            'C53 H46 Cl4 N8 O4 P2 Ru2'
_chemical_formula_weight         1264.90
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_cell_angle_alpha                90
_cell_angle_beta                 96.80(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.089(3)
_cell_length_b                   10.260(2)
_cell_length_c                   33.837(7)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    293.2
_cell_measurement_theta_max      0.0
_cell_measurement_theta_min      0.0
_cell_volume                     5546.3(19)
_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      293.2
_diffrn_measurement_device_type  'Rigaku AFC7R'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      0.01719
_diffrn_orient_matrix_UB_12      0.09260
_diffrn_orient_matrix_UB_13      -0.00456
_diffrn_orient_matrix_UB_21      -0.05834
_diffrn_orient_matrix_UB_22      0.02819
_diffrn_orient_matrix_UB_23      0.00235
_diffrn_orient_matrix_UB_31      0.01486
_diffrn_orient_matrix_UB_32      0.01160
_diffrn_orient_matrix_UB_33      0.02932
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Cu Ka'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.03786
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            6449
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         56.14
_diffrn_reflns_theta_min         2.63
_diffrn_standards_decay_%        -18.58
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.890
_exptl_absorpt_correction_T_max  0.997
_exptl_absorpt_correction_T_min  0.836
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
(North,Phillips & Matthews, 1968)
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.515
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             2552
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.62
_refine_diff_density_min         -1.09
_refine_ls_extinction_coef       0.00000017(1)
_refine_ls_extinction_expression 'equ(3) Acta Cryst.(1968) A24, p213.'
_refine_ls_extinction_method     'Zachariasen (1967)'
_refine_ls_goodness_of_fit_all   2.911
_refine_ls_goodness_of_fit_ref   3.186
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     644
_refine_ls_number_reflns         4865
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0671
_refine_ls_R_factor_gt           0.0450
_refine_ls_shift/su_max          0.3090
_refine_ls_shift/su_mean         0.1030
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00002|Fo|^2^]'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.0505
_refine_ls_wR_factor_ref         0.0490
_reflns_number_gt                4865
_reflns_number_total             6105
_reflns_threshold_expression     I>2.50\s(I)
_cod_data_source_file            b103939n.txt
_cod_data_source_block           compound
_cod_original_cell_volume        5546(2)
_cod_original_sg_symbol_H-M      'P 21/n     '
_cod_original_formula_sum        'C53 H46 Cl4 N8 O4 P2 Ru2 '
_cod_database_code               7010803