[MnBrL(CO)4] (L = Amidinatogermylene): Reductive Dimerization, Carbonyl Substitution, and Hydrolysis Reactions
Cabeza, Javier A.; García-Álvarez, Pablo; Gobetto, Roberto; González-Álvarez, Laura; Nervi, Carlo; Pérez-Carreño, Enrique; Polo, Diego; Organometallics 35 (2016) 1761–; doi:10.1021/acs.organomet.6b00168

data_4088545
_publ_section_title
;
 [MnBrL(CO)4] (L = Amidinatogermylene): Reductive Dimerization, Carbonyl
 Substitution, and Hydrolysis Reactions
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              1761
_journal_paper_doi               10.1021/acs.organomet.6b00168
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C21 H32 Br1 Ge1 Mn1 N2 O6'
_chemical_formula_sum            'C21 H32 Br Ge Mn N2 O6'
_chemical_formula_weight         615.92
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                95.819(3)
_cell_angle_beta                 104.436(3)
_cell_angle_gamma                112.043(4)
_cell_formula_units_Z            4
_cell_length_a                   10.9752(4)
_cell_length_b                   13.9014(5)
_cell_length_c                   20.2708(5)
_cell_measurement_reflns_used    10181
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      68.6810
_cell_measurement_theta_min      3.4940
_cell_volume                     2709.89(19)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'X-SEED (Barbour, 1999)'
_computing_publication_material  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SIR-97 (Giacovazzo, 1999)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Xcalibur, Onyx, Nova'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0285
_diffrn_reflns_av_unetI/netI     0.0295
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            21569
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.680
_diffrn_reflns_theta_max         69.016
_diffrn_reflns_theta_min         3.514
_diffrn_source                   'Nova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.184
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50826
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.510
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.3428
_exptl_crystal_size_mid          0.2222
_exptl_crystal_size_min          0.1495
_refine_diff_density_max         0.376
_refine_diff_density_min         -0.591
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     623
_refine_ls_number_reflns         9816
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0335
_refine_ls_R_factor_gt           0.0290
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0435P)^2^+0.6274P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0771
_refine_ls_wR_factor_ref         0.0808
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8751
_reflns_number_total             9816
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00168_si_003.cif
_cod_data_source_block           10
_cod_depositor_comments
;

2020-06-08
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_cell_volume        2709.88(17)
_cod_original_formula_moiety     '2(C21 H32 Br1 Ge1 Mn1 N2 O6)'
_cod_original_formula_sum        'C42 H64 Br2 Ge2 Mn2 N4 O12'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     1231.85
_cod_database_code               4088545
_shelxl_version_number           2014-3
_shelx_res_checksum              60300
_shelx_hkl_checksum              13624