Hydroxyl-functionalized triazolylidene-based PEPPSI complexes: metallacycle formation effect on the Suzuki coupling reaction.
Rendón-Nava, David; Álvarez-Hernández, Alejandro; Rheingold, Arnold L.; Suárez-Castillo, Oscar R; Mendoza-Espinosa, Daniel; Dalton transactions (Cambridge, England : 2003) 48 (2019) 3214–3222; doi:10.1039/c8dt04432e

data_7048609
_publ_section_title
;
 Hydroxyl-functionalized triazolylidene-based PEPPSI complexes:
 metallacycle formation effect on the Suzuki coupling reaction.
;
_journal_issue                   10
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3214
_journal_page_last               3222
_journal_paper_doi               10.1039/c8dt04432e
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety
'C19 H24 I2 N4 O Pd, C19 H19 I2 N4 O Pd, C H Cl3'
_chemical_formula_sum            'C39 H44 Cl3 I4 N8 O2 Pd2'
_chemical_formula_weight         1483.57
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-12-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-12-21 deposited with the CCDC.
2019-01-10 downloaded from the CCDC.
;
_cell_angle_alpha                79.583(2)
_cell_angle_beta                 88.011(2)
_cell_angle_gamma                88.420(2)
_cell_formula_units_Z            2
_cell_length_a                   9.8862(2)
_cell_length_b                   15.2996(4)
_cell_length_c                   17.2513(3)
_cell_measurement_reflns_used    500
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2
_cell_volume                     2564.19(10)
_computing_cell_refinement       CrisAlisPro
_computing_data_collection       'Agilent Gemini'
_computing_data_reduction        CrisAlisPro
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 'not recorded'
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0346
_diffrn_reflns_av_unetI/netI     0.0190
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            64747
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.996
_diffrn_reflns_theta_min         3.118
_exptl_absorpt_coefficient_mu    3.305
_exptl_absorpt_correction_T_max  0.590
_exptl_absorpt_correction_T_min  0.502
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.921
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1410
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.649
_refine_diff_density_min         -0.880
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     513
_refine_ls_number_reflns         9012
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0506
_refine_ls_R_factor_gt           0.0406
_refine_ls_shift/su_max          0.120
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0478P)^2^+10.9955P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1051
_refine_ls_wR_factor_ref         0.1138
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7632
_reflns_number_total             9012
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04432e2.cif
_cod_data_source_block           dm-51
_cod_depositor_comments
'Adding full bibliography for 7048608--7048609.cif.'
_cod_database_code               7048609
_shelxl_version_number           2014/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Ternary CH refined with riding coordinates:
 C39(H39)
2.b Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C4(H4A,H4B)
2.c Me refined with riding coordinates:
 C14(H14A,H14B,H14C), C13(H13A,H13B,H13C), C3(H3A,H3B,H3C), C12(H12A,H12B,
 H12C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C22(H22A,
 H22B,H22C)
2.d Aromatic/amide H refined with riding coordinates:
 C17(H17), C18(H18), C15(H15), C19(H19), C16(H16), C10(H10), C8(H8), C37(H37),
 C34(H34), C29(H29), C36(H36), C35(H35), C27(H27), C38(H38)
2.e Tetrahedral OH refined with riding coordinates:
 O1(H1)
;
_shelx_res_checksum              13796
_olex2_submission_special_instructions 'No special instructions were received'