Transition-Metal-Mediated Germanium‒Fluorine Activation: Inverse Electron Flow in σ-Bond Metathesis
Kameo, Hajime; Ikeda, Koki; Bourissou, Didier; Sakaki, Shigeyoshi; Takemoto, Shin; Nakazawa, Hiroshi; Matsuzaka, Hiroyuki; Organometallics 35 (2016) 713–; doi:10.1021/acs.organomet.5b01000

data_4088321
_publ_section_title
;
 Transition-Metal-Mediated Germanium--Fluorine Activation: Inverse
 Electron Flow in \s-Bond Metathesis
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              713
_journal_paper_doi               10.1021/acs.organomet.5b01000
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C61 H48 Ge Ir O P3, C H2 Cl2'
_chemical_formula_sum            'C62 H50 Cl2 Ge Ir O P3'
_chemical_formula_weight         1239.62
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                81.019(3)
_cell_angle_beta                 80.133(3)
_cell_angle_gamma                84.857(4)
_cell_formula_units_Z            2
_cell_length_a                   10.5656(2)
_cell_length_b                   11.1147(2)
_cell_length_c                   22.8124(5)
_cell_measurement_reflns_used    6481
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.4739
_cell_measurement_theta_min      2.0268
_cell_volume                     2601.51(9)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare <i>et al.</i>,  1999)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 7.32
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_details
;
scan:
	Number of images: 600
	           Slice: -80.0000 - 100.0000
	     Image width: 0.3000
	        Exp time: 3.0000
	   Rotation axis: Phi
	           Omega: 0.0000
	             Chi: 0.0000
	             Phi: 0.0000
	             XTD: 55.1106
	          2theta: 25.0027
scan:
	Number of images: 200
	           Slice: -15.0000 - 45.0000
	     Image width: 0.3000
	        Exp time: 3.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 90.0000
	             Phi: 0.0000
	             XTD: 55.1106
	          2theta: 25.0027
scan:
	Number of images: 200
	           Slice: -15.0000 - 45.0000
	     Image width: 0.3000
	        Exp time: 3.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 90.0000
	             Phi: 90.0000
	             XTD: 55.1106
	          2theta: 25.0027
scan:
	Number of images: 200
	           Slice: -15.0000 - 45.0000
	     Image width: 0.3000
	        Exp time: 3.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 90.0000
	             Phi: 180.0000
	             XTD: 55.1106
	          2theta: 25.0027
scan:
	Number of images: 200
	           Slice: -15.0000 - 45.0000
	     Image width: 0.3000
	        Exp time: 3.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 90.0000
	             Phi: 270.0000
	             XTD: 55.1106
	          2theta: 25.0027
scan:
	Number of images: 190
	           Slice: -15.0000 - 42.0000
	     Image width: 0.3000
	        Exp time: 3.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 0.0000
	             XTD: 55.1106
	          2theta: 25.0027
scan:
	Number of images: 190
	           Slice: -15.0000 - 42.0000
	     Image width: 0.3000
	        Exp time: 3.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 90.0000
	             XTD: 55.1106
	          2theta: 25.0027
scan:
	Number of images: 190
	           Slice: -15.0000 - 42.0000
	     Image width: 0.3000
	        Exp time: 3.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 180.0000
	             XTD: 55.1106
	          2theta: 25.0027
scan:
	Number of images: 190
	           Slice: -15.0000 - 42.0000
	     Image width: 0.3000
	        Exp time: 3.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 270.0000
	             XTD: 55.1106
	          2theta: 25.0027

;
_diffrn_measurement_device       'Mercury CCD (2x2 bin mode)'
_diffrn_measurement_device_details 'AFC7: Eulerian 3-circle'
_diffrn_measurement_device_type  'Rigaku/MSC Mercury CCD'
_diffrn_measurement_method       '\w and \f'
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0350
_diffrn_reflns_av_sigmaI/netI    0.0509
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            29984
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         2.29
_diffrn_source_current           150.0000
_diffrn_source_power             6.0000
_diffrn_source_voltage           40.0000
_exptl_absorpt_coefficient_mu    3.371
_exptl_absorpt_correction_T_max  0.6684
_exptl_absorpt_correction_T_min  0.4862
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            'Pale Yellow'
_exptl_crystal_density_diffrn    1.582
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1236
_exptl_crystal_preparation
'mounted on the CryoLoop with Palaton oil and placed in N2 stream at 200(2) K'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.711
_refine_diff_density_min         -1.009
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     641
_refine_ls_number_reflns         11468
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0348
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0249P)^2^+1.4902P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0653
_refine_ls_wR_factor_ref         0.0693
_reflns_number_gt                10236
_reflns_number_total             11468
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5b01000_si_002.cif
_cod_data_source_block           5b-trans
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4088321