Changing the Charge: Electrostatic Effects in Pd-Catalyzed Cross-Coupling
Chan, Allen L.; Estrada, Jess; Kefalidis, Christos E.; Lavallo, Vincent; Organometallics 35 (2016) 3257–; doi:10.1021/acs.organomet.6b00622

data_4088993
_publ_section_title
;
 Changing the Charge: Electrostatic Effects in Pd-Catalyzed Cross-Coupling
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              3257
_journal_paper_doi               10.1021/acs.organomet.6b00622
_journal_volume                  35
_journal_year                    2016
_chemical_formula_sum            'C30 H81 B22 Li O4 P2 Pd'
_chemical_formula_weight         919.04
_space_group_crystal_system      monoclinic
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_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 93.7182(18)
_cell_angle_gamma                90
_cell_formula_units_Z            8
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_cell_length_b                   8.3209(11)
_cell_length_c                   59.641(7)
_cell_measurement_reflns_used    9977
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.00
_cell_measurement_theta_min      2.23
_cell_volume                     10051(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
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_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.760
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0792
_diffrn_reflns_av_unetI/netI     0.1193
_diffrn_reflns_Laue_measured_fraction_full 0.760
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       55
_diffrn_reflns_limit_l_min       -65
_diffrn_reflns_number            34843
_diffrn_reflns_point_group_measured_fraction_full 0.760
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         23.257
_diffrn_reflns_theta_min         1.645
_exptl_absorpt_coefficient_mu    0.466
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.215
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'thin needle frag'
_exptl_crystal_F_000             3856
_exptl_crystal_size_max          0.545
_exptl_crystal_size_mid          0.096
_exptl_crystal_size_min          0.046
_exptl_transmission_factor_max   0.958
_exptl_transmission_factor_min   0.543
_refine_diff_density_max         1.375
_refine_diff_density_min         -0.959
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
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_refine_ls_number_reflns         13797
_refine_ls_number_restraints     1899
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.1300
_refine_ls_R_factor_gt           0.0810
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0585P)^2^+30.3440P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1612
_refine_ls_wR_factor_ref         0.1776
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9096
_reflns_number_total             13797
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00622_si_002.cif
_cod_data_source_block           Compound_6
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4088993
_shelx_estimated_absorpt_t_min   0.785
_shelx_estimated_absorpt_t_max   0.979
_shelxl_version_number           2013-4
_shelx_res_checksum              44783
_shelx_hkl_checksum              22405