Evaluation of P-bridged biaryl phosphine ligands in palladium-catalysed Suzuki–Miyaura cross-coupling reactions
Lamola, Jairus L.; Moshapo, Paseka T.; Holzapfel, Cedric W.; Maumela, Munaka Christopher; RSC Advances 11 (2021) 26883–26891; doi:10.1039/D1RA04947J

data_7243351
_publ_section_title
;
 Evaluation of P-bridged biaryl phosphine ligands in palladium-catalysed
 Suzuki--Miyaura cross-coupling reactions
;
_journal_issue                   43
_journal_name_full               'RSC Advances'
_journal_page_first              26883
_journal_page_last               26891
_journal_paper_doi               10.1039/D1RA04947J
_journal_volume                  11
_journal_year                    2021
_chemical_formula_moiety         'C20 H23 P'
_chemical_formula_sum            'C20 H23 P'
_chemical_formula_weight         294.38
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2020-12-06
_audit_creation_method
;
Olex2 1.3
(compiled 2019.09.11 svn.r3662 for OlexSys, GUI svn.r5938)
;
_audit_update_record
;
2020-12-22 deposited with the CCDC.	2021-07-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.878(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.554(2)
_cell_length_b                   7.2220(11)
_cell_length_c                   31.176(4)
_cell_measurement_reflns_used    9909
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.99
_cell_measurement_theta_min      2.639
_cell_volume                     3246.0(8)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_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  0.0476
_diffrn_reflns_av_unetI/netI     0.0342
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            37990
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.088
_diffrn_reflns_theta_min         2.584
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.936
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.5784
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'clear whiteish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.620
_exptl_crystal_description       plate
_exptl_crystal_F_000             1584
_exptl_crystal_preparation       Methanol
_exptl_crystal_size_max          0.134
_exptl_crystal_size_mid          0.094
_exptl_crystal_size_min          0.071
_refine_diff_density_max         0.631
_refine_diff_density_min         -0.219
_refine_diff_density_rms         0.042
_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     379
_refine_ls_number_reflns         6384
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0495
_refine_ls_R_factor_gt           0.0413
_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^)+(0.0314P)^2^+1.9667P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0942
_refine_ls_wR_factor_ref         0.0980
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5509
_reflns_number_total             6384
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ra04947j2.cif
_cod_data_source_block           mo_20bv_l1_173k_solve_a
_cod_depositor_comments
;

2025-01-31
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C40 H46 P2'
_cod_original_formula_weight         588.76
_cod_original_formula_moiety         '2(C20 H23 P)'
_cod_original_formula_units_Z            72
_cod_database_code               7243351
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Ternary CH refined with riding coordinates:
 C00D(H00R), C00F(H00F), C00L(H00W), C00M(H00M)
2.b Secondary CH2 refined with riding coordinates:
 C00H(H00A,H00B), C00P(H00D,H00E), C00R(H00Z,H), C00S(H00,HA), C00T(H00H,H00I),
  C00W(H00K,H00L), C00X(H2,HB), C00Y(H3,HC), C00Z(H00N,H00O), C010(H01A,H01B),
 C014(H01C,H01D), C016(H01E,H01F)
2.c Aromatic/amide H refined with riding coordinates:
 C005(H005), C006(H006), C00B(H00P), C00C(H00C), C00E(H00S), C00G(H00G),
 C00I(H00T), C00J(H00J), C00K(H00V), C00N(H00X), C00O(H00Y), C00Q(H00Q),
 C00U(H00U), C00V(H1), C011(H011), C012(H012), C013(H013), C015(H015)
;
_shelx_res_checksum              94625
_olex2_submission_special_instructions 'No special instructions were received'