Preparation, characterization and reactivity of trifluoromethoxy palladium(ii) complexes
Xu, Songsong; Shao, Yingbo; Zheng, Hanliang; Leng, Xuebing; Xue, Xiao-Song; Shen, Qilong; New Journal of Chemistry 46 (2022) 20760–20767; doi:10.1039/D2NJ04198G

data_7061945
_publ_section_title
;
 Preparation, characterization and reactivity of trifluoromethoxy
 palladium(ii) complexes
;
_journal_issue                   43
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              20760
_journal_page_last               20767
_journal_paper_doi               10.1039/D2NJ04198G
_journal_volume                  46
_journal_year                    2022
_chemical_formula_moiety         'C47 H39 F3 Fe N P2 Pd, C7 H8'
_chemical_formula_sum            'C54 H47 F3 Fe N P2 Pd'
_chemical_formula_weight         991.11
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-09-15
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-09-25 deposited with the CCDC.	2022-09-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.5760(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.3574(2)
_cell_length_b                   17.7893(3)
_cell_length_c                   27.4578(5)
_cell_measurement_reflns_used    9939
_cell_measurement_temperature    169.96
_cell_measurement_theta_max      54.812
_cell_measurement_theta_min      3.550
_cell_volume                     5035.19(16)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      169.96
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0553
_diffrn_reflns_av_unetI/netI     0.0359
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            65307
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         54.976
_diffrn_reflns_theta_min         3.548
_diffrn_source_current           2.86
_diffrn_source_power             0.1995708
_diffrn_source_voltage           69.78
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.112
_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.4841
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1705 before and 0.0659 after correction. The Ratio of minimum to maximum transmission is 0.6448. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_description       block
_exptl_crystal_F_000             2028
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.529
_refine_diff_density_min         -0.736
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     561
_refine_ls_number_reflns         9567
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0548
_refine_ls_R_factor_gt           0.0415
_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^)+(0.0547P)^2^+5.5692P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1014
_refine_ls_wR_factor_ref         0.1087
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7756
_reflns_number_total             9567
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj04198g2.cif
_cod_data_source_block           mj19744_0m
_cod_depositor_comments
'Adding full bibliography for 7061942--7061946.cif.'
_cod_database_code               7061945
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.821
_shelx_estimated_absorpt_t_min   0.734
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C54(H54), C3(H3), C5(H5), C6(H6), C8(H8), C9(H9), C11(H11), C12(H12),
 C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21), C22(H22), C23(H23),
  C25(H25), C26(H26), C27(H27), C28(H28), C29(H29), C31(H31), C32(H32),
 C33(H33), C34(H34), C35(H35), C37(H37), C38(H38), C39(H39), C40(H40), C41(H41),
  C43(H43), C44(H44), C45(H45), C46(H46), C47(H47), C2(H2), C48(H48), C49(H49),
 C51(H51), C52(H52)
2.b Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C53(H53A,H53B,H53C)
;
_shelx_res_checksum              81785
_shelx_fab_checksum              45324
_olex2_submission_special_instructions 'No special instructions were received'