Phenylcyanamidoruthenium Scorpionate Complexes
Carmen Harb; Pavel Kravtsov; Mohommad Choudhuri; Eric R. Sirianni; Glenn P. A. Yap; A. B. P. Lever; Robert J. Crutchley; Inorganic Chemistry 52 (2013) 1621–1630; doi:10.1021/ic302535h

data_4333759
_publ_section_title
;
 Phenylcyanamidoruthenium Scorpionate Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1621
_journal_page_last               1630
_journal_paper_doi               10.1021/ic302535h
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C84 H76 B2 N18 P4 Ru2, 2(O H2)'
_chemical_formula_sum            'C84 H80 B2 N18 O2 P4 Ru2'
_chemical_formula_weight         1721.30
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 109.513(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.035(3)
_cell_length_b                   25.181(6)
_cell_length_c                   15.913(4)
_cell_measurement_reflns_used    1003
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      17.36
_cell_measurement_theta_min      2.42
_cell_volume                     4545.5(19)
_computing_cell_refinement       'SAINT (Bruker, 2002)'
_computing_data_collection       'SMART (Bruker, 2002)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2001)'
_computing_publication_material  'SHELXTL (Sheldrick, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 836.6
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker AXS APEX diffractometer'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1302
_diffrn_reflns_av_sigmaI/netI    0.1125
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            47731
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.11
_diffrn_standards_decay_%        1
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.456
_exptl_absorpt_correction_T_max  0.9878
_exptl_absorpt_correction_T_min  0.9306
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2003)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.258
_exptl_crystal_description       plate
_exptl_crystal_F_000             1768
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.03
_platon_squeeze_details
;

- PLATON Reference : Spek, A.L. (2003), J.Appl.Cryst. 36, 7-13

Void space analysis consistent with initial solutions suggesting
two water molecules of hydration per diruthenium molecule.
;
_refine_diff_density_max         0.596
_refine_diff_density_min         -0.319
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     499
_refine_ls_number_reflns         8006
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.1280
_refine_ls_R_factor_gt           0.0685
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0393P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1211
_refine_ls_wR_factor_ref         0.1393
_reflns_number_gt                4593
_reflns_number_total             8006
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302535h_si_001.cif
_cod_data_source_block           bobr008s
_cod_original_cell_volume        4545.3(18)
_cod_database_code               4333759