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_7047731
_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         'C33 H57 Cl2 Ge Ir N2 O Si2'
_chemical_formula_sum            'C33 H57 Cl2 Ge Ir N2 O Si2'
_chemical_formula_weight         889.67
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yab'
_space_group_name_H-M_alt        'P 1 21/a 1'
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-05-02
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-05-02 deposited with the CCDC.
2018-10-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.867(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.1906(13)
_cell_length_b                   11.1401(7)
_cell_length_c                   24.7705(17)
_cell_measurement_reflns_used    8002
_cell_measurement_temperature    150
_cell_measurement_theta_max      29.2029
_cell_measurement_theta_min      3.8579
_cell_volume                     4514.9(6)
_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      150
_diffrn_detector_area_resol_mean 15.9821
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.849
_diffrn_measurement_details
;
  1 omega  -22.00   50.00   1.0000    9.6600
omega____ theta____ kappa____ phi______ frames
    -      -17.8085   57.0000  120.0000 72

  2 omega  -86.00  -22.00   1.0000    9.6600
omega____ theta____ kappa____ phi______ frames
    -      -17.8085  -57.0000  -30.0000 64

  3 omega  -64.00   -6.00   1.0000    9.6600
omega____ theta____ kappa____ phi______ frames
    -      -17.8085  -37.0000    0.0000 58

  4 omega  -24.00    3.00   1.0000    9.6600
omega____ theta____ kappa____ phi______ frames
    -      -17.8085  -99.0000  -60.0000 27

  5 omega  -37.00  -10.00   1.0000    9.6600
omega____ theta____ kappa____ phi______ frames
    -      -17.8085  109.0000 -141.0000 27

  6 omega  -33.00   -6.00   1.0000    9.6600
omega____ theta____ kappa____ phi______ frames
    -      -17.8085  -77.0000 -180.0000 27

  7 omega  -11.00   24.00   1.0000    9.6600
omega____ theta____ kappa____ phi______ frames
    -      -17.8085  -99.0000  -30.0000 35
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0287863000
_diffrn_orient_matrix_UB_12      0.0151898000
_diffrn_orient_matrix_UB_13      -0.0141383000
_diffrn_orient_matrix_UB_21      0.0322085000
_diffrn_orient_matrix_UB_22      -0.0061427000
_diffrn_orient_matrix_UB_23      0.0258498000
_diffrn_orient_matrix_UB_31      0.0037915000
_diffrn_orient_matrix_UB_32      -0.0615635000
_diffrn_orient_matrix_UB_33      -0.0061030000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0645
_diffrn_reflns_av_unetI/netI     0.0792
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.849
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            25379
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.849
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.258
_diffrn_reflns_theta_min         3.864
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.805
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.17790
_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 red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.309
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1792
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.57
_exptl_crystal_size_min          0.09
_refine_diff_density_max         4.159
_refine_diff_density_min         -4.790
_refine_diff_density_rms         0.283
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     395
_refine_ls_number_reflns         10442
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0935
_refine_ls_R_factor_gt           0.0759
_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^)+(0.1542P)^2^+16.6901P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2126
_refine_ls_wR_factor_ref         0.2330
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8298
_reflns_number_total             10442
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03166e2.cif
_cod_data_source_block           ndr-brg-ir-1-s
_cod_depositor_comments
'Adding full bibliography for 7047730--7047732.cif.'
_cod_database_code               7047731
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C56 H44 Ir1 N4 O20'
_chemical_oxdiff_usercomment     'RED COLOUR PLATE, 230K, 0.75 0.75 0.06'
_shelx_estimated_absorpt_t_max   0.726
_shelx_estimated_absorpt_t_min   0.209
_reflns_odcompleteness_completeness 98.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C3(H3), C4(H4)
2.b Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B)
2.c Aromatic/amide H refined with riding coordinates:
 N1(H1), C15(H15), C9(H9), C11(H11), C10(H10)
2.d Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C24(H24A,H24B,H24C), C2(H2A,H2B,H2C), C26(H26A,H26B,
 H26C), C29(H29A,H29B,H29C), C23(H23A,H23B,H23C), C33(H33A,H33B,H33C), C1(H1A,
 H1B,H1C), C32(H32A,H32B,H32C), C27(H27A,H27B,H27C), C30(H30A,H30B,H30C),
 C13(H13A,H13B,H13C), C28(H28A,H28B,H28C), C6(H6A,H6B,H6C), C25(H25A,H25B,H25C),
  C5(H5A,H5B,H5C)
;
_shelx_res_checksum              95303
_shelx_fab_checksum              93765
_olex2_submission_special_instructions 'No special instructions were received'