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_7061946
_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, C F3 O3 S'
_chemical_formula_sum            'C48 H39 F6 Fe N O3 P2 Pd S'
_chemical_formula_weight         1048.05
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-06-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-09-26 deposited with the CCDC.	2022-09-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.6907(5)
_cell_length_b                   17.7028(4)
_cell_length_c                   22.6847(5)
_cell_measurement_reflns_used    9936
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      46.79
_cell_measurement_theta_min      3.28
_cell_volume                     8710.6(3)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      213.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0699
_diffrn_reflns_av_unetI/netI     0.0334
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            88491
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         54.877
_diffrn_reflns_theta_min         3.276
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.205
_exptl_absorpt_correction_T_max  0.7510
_exptl_absorpt_correction_T_min  0.5513
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1889 before and 0.0634 after correction. The Ratio of minimum to maximum transmission is 0.6324. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.598
_exptl_crystal_description       block
_exptl_crystal_F_000             4240
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.467
_refine_diff_density_min         -0.784
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     587
_refine_ls_number_reflns         8247
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_gt           0.0348
_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^)+(0.0360P)^2^+10.7823P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0844
_refine_ls_wR_factor_ref         0.0896
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6885
_reflns_number_total             8247
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj04198g2.cif
_cod_data_source_block           mj22132
_cod_depositor_comments
'Adding full bibliography for 7061942--7061946.cif.'
_cod_database_code               7061946
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.781
_shelx_estimated_absorpt_t_min   0.712
_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
2. Shared sites
{C1A, N1}
{C2A, N2}
3. Rigid bond restraints
 C18, F3, C18, F2, C18, F1, C24, F4, C24, F5, C24, F6
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
C18 \\sim F3 \\sim F2 \\sim F1: within 2A with sigma of 0.005 and sigma for
terminal atoms of 0.01
C24 \\sim F4 \\sim F5 \\sim F6: within 2A with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uiso(C1A) = Uiso(N1)
Uiso(N1) = Uiso(C1A)
Uiso(C2A) = Uiso(N2)
5. Others
 Fixed Sof: F1(0.5) F2(0.5) F3(0.5) F4(0.5) F5(0.5) F6(0.5) N1(0.5) N2(0.5)
 H13(0.5) H13A(0.5) H17(0.5) H17A(0.5) H18A(0.5) H18B(0.5) H18C(0.5) H19(0.5)
 H19A(0.5) H23(0.5) H23A(0.5) H24C(0.5) H24A(0.5) H24B(0.5) C1A(0.5) C2A(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C13(H13A), C14(H14), C16(H16), C17(H17), C17(H17A), C19(H19),
 C19(H19A), C20(H20), C22(H22), C23(H23), C23(H23A), C26(H26), C27(H27),
 C28(H28), C29(H29), C30(H30), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36),
  C38(H38), C39(H39), C40(H40), C41(H41), C42(H42), C44(H44), C45(H45),
 C46(H46), C47(H47), C48(H48)
6.b Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C24(H24C,H24A,H24B)
;
_shelx_res_checksum              21884
_olex2_submission_special_instructions 'No special instructions were received'