[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_4088544
_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         'C25 H37 Br Ge Mn N3 O3'
_chemical_formula_sum            'C25 H37 Br Ge Mn N3 O3'
_chemical_formula_weight         635.01
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 92.705(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.456(2)
_cell_length_b                   16.545(4)
_cell_length_c                   18.540(4)
_cell_measurement_reflns_used    1935
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28,045
_cell_measurement_theta_min      2,2
_cell_volume                     2897.3(11)
_computing_cell_refinement
;
'SMART: Bruker Molecular Analysis Research Tool V5.054 Copyr. 1997-98 Bruker
AXS.'
;
_computing_data_collection
;
'SMART: Bruker Molecular Analysis Research Tool V5.054 Copyr. 1997-98 Bruker
AXS.'
;
_computing_data_reduction
;
'SMART: Bruker Molecular Analysis Research Tool V5.054 Copyr. 1997-98 Bruker
AXS.'
;
_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      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker CCD SMART1000'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0557
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            6890
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.480
_diffrn_reflns_theta_min         2.199
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.881
_exptl_absorpt_correction_T_max  0.8491
_exptl_absorpt_correction_T_min  0.6183
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56
Cubic fit to sin(theta)/lambda - 24 parameters
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.456
_exptl_crystal_description       plate
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.310
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.090
_refine_diff_density_max         0.378
_refine_diff_density_min         -0.414
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details
;
 Flack x determined using 2823 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.005(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     321
_refine_ls_number_reflns         6657
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0360
_refine_ls_R_factor_gt           0.0312
_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^)+(0.0277P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0680
_refine_ls_wR_factor_ref         0.0698
_reflns_Friedel_coverage         0.994
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                6145
_reflns_number_total             6657
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00168_si_003.cif
_cod_data_source_block           9
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               4088544
_shelx_estimated_absorpt_t_min   0.469
_shelx_estimated_absorpt_t_max   0.782
_shelxl_version_number           2014-3
_shelx_res_checksum              48349
_shelx_hkl_checksum              95914