Pd/Ni-Catalyzed Germa-Suzuki coupling <i>via</i> dual Ge-F bond activation.
Kameo, Hajime; Mushiake, Akihiro; Isasa, Tomohito; Matsuzaka, Hiroyuki; Bourissou, Didier; Chemical communications (Cambridge, England) 57 (2021) 5004–5007; doi:10.1039/d1cc01392k

data_7128196
_publ_section_title
;
 Pd/Ni-Catalyzed Germa-Suzuki coupling <i>via</i> dual Ge-F bond
 activation.
;
_journal_issue                   41
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              5004
_journal_page_last               5007
_journal_paper_doi               10.1039/d1cc01392k
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C60 H48 F Ge P3 Pd, 2(C6 H6)'
_chemical_formula_sum            'C72 H60 F Ge P3 Pd'
_chemical_formula_weight         1216.10
_chemical_properties_physical    Air-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_audit_creation_date             2020-5-25
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-12-11 deposited with the CCDC.	2021-04-20 downloaded from the CCDC.
;
_cell_angle_alpha                109.543(5)
_cell_angle_beta                 96.454(2)
_cell_angle_gamma                98.884(3)
_cell_formula_units_Z            2
_cell_length_a                   13.3586(12)
_cell_length_b                   14.0431(16)
_cell_length_c                   16.711(2)
_cell_measurement_reflns_used    3613
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.4546
_cell_measurement_theta_min      2.4375
_cell_volume                     2873.2(6)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 7.111
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_details
;
scan:
	Number of images: 360
	           Slice: -115.0000 - 65.0000
	     Image width: 0.5000
	        Exp time: 1.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 0.0000
	             XTD: 54.9531
	          2theta: -25.3721
scan:
	Number of images: 360
	           Slice: -115.0000 - 65.0000
	     Image width: 0.5000
	        Exp time: 1.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 90.0000
	             XTD: 54.9531
	          2theta: -25.3721
scan:
	Number of images: 360
	           Slice: -115.0000 - 65.0000
	     Image width: 0.5000
	        Exp time: 1.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 180.0000
	             XTD: 54.9531
	          2theta: -25.3721

;
_diffrn_measurement_device       'Saturn724+ (4x4 bin mode)'
_diffrn_measurement_device_details 'AFC11 (Right): Eulerian 3 circle'
_diffrn_measurement_device_type  'Rigaku AFC11 with Saturn 724+ CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.710747
_diffrn_reflns_av_R_equivalents  0.0320
_diffrn_reflns_av_unetI/netI     0.0577
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            22527
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.444
_diffrn_reflns_theta_min         2.383
_diffrn_source_current           24.0000
_diffrn_source_power             1.2000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    0.967
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9165
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1248
_exptl_crystal_preparation
'mounted on the CryoLoop with Palaton oil and placed in N2 stream at 200(2) K'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Benzene / Pentane'
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.644
_refine_diff_density_min         -0.585
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     679
_refine_ls_number_reflns         12713
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0614
_refine_ls_R_factor_gt           0.0496
_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^)+(0.0329P)^2^+3.3019P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0955
_refine_ls_wR_factor_ref         0.1033
_reflns_number_gt                10685
_reflns_number_total             12713
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc01392k2.cif
_cod_data_source_block           PdGermane
_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/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/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 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7128196--7128199.cif.
;
_cod_original_cell_volume        2873.2(5)
_cod_database_code               7128196
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.830
_shelx_estimated_absorpt_t_max   0.927
_shelx_res_checksum              23592
_shelx_hkl_checksum              73030