Amidinatogermylene derivatives of ruthenium carbonyl: new insights into the reactivity of [Ru3(CO)12] with two-electron-donor reagents of high basicity.
Álvarez-Rodríguez, Lucía; Cabeza, Javier A.; García-Álvarez, Pablo; Pérez-Carreño, Enrique; Polo, Diego; Inorganic chemistry 54 (2015) 2983–2994; doi:10.1021/acs.inorgchem.5b00084

data_4346041
_publ_section_title
;
 Amidinatogermylene derivatives of ruthenium carbonyl: new insights into
 the reactivity of [Ru3(CO)12] with two-electron-donor reagents of high
 basicity.
;
_journal_issue                   6
_journal_name_full               'Inorganic chemistry'
_journal_page_first              2983
_journal_page_last               2994
_journal_paper_doi               10.1021/acs.inorgchem.5b00084
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C60 H84 Ge3 N6 O9 Ru3, C7 H8'
_chemical_formula_sum            'C67 H92 Ge3 N6 O9 Ru3'
_chemical_formula_weight         1646.44
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.6511(2)
_cell_length_b                   17.8306(2)
_cell_length_c                   26.7297(4)
_cell_measurement_temperature    133(2)
_cell_volume                     7459.42(17)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_molecular_graphics    'MERCUY CSD 3.1 (Build RC5)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR-97 (Giacovazzo, 1999)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Xcalibur, Onyx, Nova'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0344
_diffrn_reflns_av_unetI/netI     0.0485
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            21310
_diffrn_reflns_point_group_measured_fraction_full 0.906
_diffrn_reflns_point_group_measured_fraction_max 0.916
_diffrn_reflns_theta_full        70.000
_diffrn_reflns_theta_max         69.432
_diffrn_reflns_theta_min         3.272
_diffrn_source                   'Nova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.592
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88813
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.466
_exptl_crystal_description       fragment
_exptl_crystal_F_000             3344
_exptl_crystal_size_max          0.1984
_exptl_crystal_size_mid          0.1193
_exptl_crystal_size_min          0.1115
_refine_diff_density_max         0.477
_refine_diff_density_min         -0.493
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details
;
 Flack x determined using 4690 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.025(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     841
_refine_ls_number_reflns         12820
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0329
_refine_ls_R_factor_gt           0.0287
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0279P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0655
_refine_ls_wR_factor_ref         0.0685
_reflns_Friedel_coverage         0.708
_reflns_Friedel_fraction_full    0.829
_reflns_Friedel_fraction_max     0.839
_reflns_number_gt                11908
_reflns_number_total             12820
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b00084_si_002.cif
_cod_data_source_block           6ipr
_cod_database_code               4346041
_shelxl_version_number           2014-3
_shelx_res_checksum              84991
_shelx_hkl_checksum              3922