Conversion of a Monodentate Amidinate-Germylene Ligand into Chelating Imine-Germanate Ligands (on Mononuclear Manganese Complexes).
Cabeza, Javier A.; García-Álvarez, Pablo; Pérez-Carreño, Enrique; Polo, Diego; Inorganic chemistry 53 (2014) 8735–8741; doi:10.1021/ic501418p

data_4340792
_publ_section_title
;
 Conversion of a Monodentate Amidinate-Germylene Ligand into Chelating
 Imine-Germanate Ligands (on Mononuclear Manganese Complexes).
;
_journal_issue                   16
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8735
_journal_page_last               8741
_journal_paper_doi               10.1021/ic501418p
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C22 H31 Ge Mn N2 O4'
_chemical_formula_sum            'C22 H31 Ge Mn N2 O4'
_chemical_formula_weight         515.02
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.098(4)
_cell_length_b                   14.182(2)
_cell_length_c                   9.9035(19)
_cell_measurement_reflns_used    433
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      50.6230
_cell_measurement_theta_min      5.1580
_cell_volume                     2401.4(8)
_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    '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      123(10)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.2997
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            2792
_diffrn_reflns_theta_full        64.97
_diffrn_reflns_theta_max         64.97
_diffrn_reflns_theta_min         4.05
_exptl_absorpt_coefficient_mu    6.055
_exptl_absorpt_correction_T_max  0.2729
_exptl_absorpt_correction_T_min  0.0926
_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            colourless
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.1165
_exptl_crystal_size_mid          0.0754
_exptl_crystal_size_min          0.0361
_refine_diff_density_max         0.645
_refine_diff_density_min         -0.573
_refine_diff_density_rms         0.107
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.957
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     268
_refine_ls_number_reflns         2792
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.957
_refine_ls_R_factor_all          0.1812
_refine_ls_R_factor_gt           0.0923
_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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1903
_refine_ls_wR_factor_ref         0.2904
_reflns_number_gt                1128
_reflns_number_total             2792
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic501418p_si_002.cif
_cod_data_source_block           gmn13078_dp446
_cod_depositor_comments
'Adding full bibliography for 4340791--4340795.cif.'
_cod_database_code               4340792