Cyclometallation of a germylene ligand by concerted metalation-deprotonation of a methyl group.
Bakthavachalam, K.; Dutta, Sayan; C, Arivazhagan; Raghavendra, Beesam; Haridas, Anagha; Sen, Sakya S.; Koley, Debasis; Ghosh, Sundargopal; Dalton transactions (Cambridge, England : 2003) 47 (2018) 15835–15844; doi:10.1039/c8dt03166e

data_7047730
_publ_section_title
;
 Cyclometallation of a germylene ligand by concerted
 metalation-deprotonation of a methyl group.
;
_journal_issue                   44
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15835
_journal_page_last               15844
_journal_paper_doi               10.1039/c8dt03166e
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C17 H24 Cl Ge N O'
_chemical_formula_sum            'C17 H24 Cl Ge N O'
_chemical_formula_weight         366.41
_space_group_crystal_system      trigonal
_space_group_IT_number           145
_space_group_name_Hall           'P 32'
_space_group_name_H-M_alt        'P 32'
_symmetry_space_group_name_Hall  'P 32'
_symmetry_space_group_name_H-M   'P 32'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-05-03
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-05-03 deposited with the CCDC.
2018-10-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   12.2217(5)
_cell_length_b                   12.2217(5)
_cell_length_c                   10.6077(7)
_cell_measurement_reflns_used    1510
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      29.1038
_cell_measurement_theta_min      3.8425
_cell_volume                     1372.19(12)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 15.9821
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.868
_diffrn_measurement_details
;
  1 omega  -88.00  -60.00   1.0000   11.9900
omega____ theta____ kappa____ phi______ frames
    -      -17.4178 -178.0000  150.0000 28

  2 omega  -73.00  -43.00   1.0000   11.9900
omega____ theta____ kappa____ phi______ frames
    -      -17.4178  -19.0000   30.0000 30

  3 omega  -18.00   22.00   1.0000   11.9900
omega____ theta____ kappa____ phi______ frames
    -      -17.4178  -19.0000   30.0000 40

  4 omega  -81.00   -2.00   1.0000   11.9900
omega____ theta____ kappa____ phi______ frames
    -      -17.4178  -57.0000 -180.0000 79

  5 omega  -24.00    1.00   1.0000   11.9900
omega____ theta____ kappa____ phi______ frames
    -      -17.4178  -99.0000  -90.0000 25
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0346778000
_diffrn_orient_matrix_UB_12      0.0259034000
_diffrn_orient_matrix_UB_13      0.0281215000
_diffrn_orient_matrix_UB_21      -0.0051210000
_diffrn_orient_matrix_UB_22      -0.0332875000
_diffrn_orient_matrix_UB_23      0.0565225000
_diffrn_orient_matrix_UB_31      0.0571020000
_diffrn_orient_matrix_UB_32      0.0520713000
_diffrn_orient_matrix_UB_33      0.0220955000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0390
_diffrn_reflns_av_unetI/netI     0.0662
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.868
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5344
_diffrn_reflns_point_group_measured_fraction_full 0.872
_diffrn_reflns_point_group_measured_fraction_max 0.720
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         29.168
_diffrn_reflns_theta_min         3.850
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.819
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66179
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.330
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             570
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.501
_refine_diff_density_min         -0.486
_refine_diff_density_rms         0.059
_refine_ls_abs_structure_details
;
 Flack x determined using 925 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.003(18)
_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     196
_refine_ls_number_reflns         3555
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0687
_refine_ls_R_factor_gt           0.0497
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0580P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1088
_refine_ls_wR_factor_ref         0.1235
_reflns_Friedel_coverage         0.657
_reflns_Friedel_fraction_full    0.750
_reflns_Friedel_fraction_max     0.571
_reflns_number_gt                2793
_reflns_number_total             3555
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03166e2.cif
_cod_data_source_block           ndr-brg-gei-g
_cod_depositor_comments
'Adding full bibliography for 7047730--7047732.cif.'
_cod_original_cell_volume        1372.20(15)
_cod_database_code               7047730
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C21 H9 N4 O3 Ge1'
_chemical_oxdiff_usercomment     'COLOURLESS PLATE, 298K, 0.65 0.6 0.08'
_shelx_estimated_absorpt_t_max   0.868
_shelx_estimated_absorpt_t_min   0.384
_reflns_odcompleteness_completeness 99.31
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C16(H16), C13(H13)
2.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C11(H11), C3(H3)
2.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C14(H14A,H14B,H14C),
 C17(H17A,H17B,H17C), C15(H15A,H15B,H15C)
;
_shelx_res_checksum              8032
_olex2_submission_special_instructions 'No special instructions were received'