Structure-Modified Germatranes for Pd-Catalyzed Biaryl Synthesis
Song, Hai-Jie; Jiang, Wei-Tao; Zhou, Qiao-Lan; Xu, Meng-Yu; Xiao, Bin; ACS Catalysis 8 (2018) 9287–; doi:10.1021/acscatal.8b02661

data_4515543
_publ_section_title
;
 Structure-Modified Germatranes for Pd-Catalyzed Biaryl Synthesis
;
_journal_issue                   10
_journal_name_full               'ACS Catalysis'
_journal_page_first              9287
_journal_paper_doi               10.1021/acscatal.8b02661
_journal_volume                  8
_journal_year                    2018
_chemical_formula_sum            'C14 H20 Cl Ge N O3'
_chemical_formula_weight         358.35
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 96.777(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.8342(3)
_cell_length_b                   13.3798(3)
_cell_length_c                   16.4653(4)
_cell_measurement_reflns_used    6107
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      71.3480
_cell_measurement_theta_min      3.7880
_cell_volume                     3245.18(13)
_computing_cell_refinement       'CrysAlisPro (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro (Rigaku OD, 2015)'
_computing_molecular_graphics    'Ortep-3 (L. J. Farrugia, 2001)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(1)
_diffrn_detector_area_resol_mean 5.2169
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0368
_diffrn_reflns_av_unetI/netI     0.0450
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            12642
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.288
_diffrn_reflns_theta_min         3.795
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    4.138
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49096
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_description       block
_exptl_crystal_F_000             1472
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.200
_platon_squeeze_details
;
;
_refine_diff_density_max         1.419
_refine_diff_density_min         -0.807
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     369
_refine_ls_number_reflns         6131
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0500
_refine_ls_R_factor_gt           0.0421
_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^)+(0.0610P)^2^+1.5884P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1081
_refine_ls_wR_factor_ref         0.1132
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5150
_reflns_number_total             6131
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs8b02661_si_001.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
;

2020-05-08
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C28 H40 Cl2 Ge2 N2 O6'
_cod_original_formula_weight         716.70
_cod_original_formula_units_Z            4
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4515543
_shelx_estimated_absorpt_t_min   0.424
_shelx_estimated_absorpt_t_max   0.492
_shelxl_version_number           2013-4
_shelx_res_checksum              26122
_shelx_hkl_checksum              67368