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_4346040
_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_sum            'C30 H32 Ge N2 O11 Ru3'
_chemical_formula_weight         972.37
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 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                   17.3399(3)
_cell_length_b                   9.1771(2)
_cell_length_c                   22.6692(4)
_cell_measurement_reflns_used    11888
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.7800
_cell_measurement_theta_min      3.5760
_cell_volume                     3607.35(12)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_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      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0460
_diffrn_reflns_av_unetI/netI     0.0461
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            25081
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.994
_diffrn_reflns_theta_min         3.232
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.114
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98213
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.790
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1912
_exptl_crystal_size_max          0.1676
_exptl_crystal_size_mid          0.0984
_exptl_crystal_size_min          0.0688
_refine_diff_density_max         0.417
_refine_diff_density_min         -0.329
_refine_diff_density_rms         0.075
_refine_ls_abs_structure_details
;
 Flack x determined using 2962 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.004(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         6999
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0299
_refine_ls_R_factor_gt           0.0261
_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^)+(0.0105P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0414
_refine_ls_wR_factor_ref         0.0429
_reflns_Friedel_coverage         0.932
_reflns_Friedel_fraction_full    0.982
_reflns_Friedel_fraction_max     0.982
_reflns_number_gt                6588
_reflns_number_total             6999
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b00084_si_002.cif
_cod_data_source_block           4tBu
_cod_database_code               4346040
_shelxl_version_number           2014-3
_shelx_res_checksum              24433
_shelx_hkl_checksum              33599