Fluxional chloro-pyrrole‒Pd(ii) complex to cationic η2-pyrrole‒Pd(ii) complex: subtlety in structure-directed bonding mode
Saha, Debajyoti; Sepay, Nayim; New Journal of Chemistry 45 (2021) 10594–10598; doi:10.1039/D1NJ00866H

data_7060692
_publ_section_title
;
 Fluxional chloro-pyrrole--Pd(ii) complex to cationic \h2-pyrrole--Pd(ii)
 complex: subtlety in structure-directed bonding mode
;
_journal_issue                   24
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              10594
_journal_page_last               10598
_journal_paper_doi               10.1039/D1NJ00866H
_journal_volume                  45
_journal_year                    2021
_chemical_formula_moiety         'C27 H27 N P Pd, F6.174 Sb'
_chemical_formula_sum            'C27 H27 F6.18 N P Pd Sb'
_chemical_formula_weight         741.94
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-05-12
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-05-12 deposited with the CCDC.	2021-05-18 downloaded from the CCDC.
;
_cell_angle_alpha                89.114(2)
_cell_angle_beta                 75.267(2)
_cell_angle_gamma                81.910(2)
_cell_formula_units_Z            2
_cell_length_a                   8.9132(8)
_cell_length_b                   11.1285(10)
_cell_length_c                   14.9029(14)
_cell_measurement_reflns_used    9213
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.51
_cell_measurement_theta_min      2.30
_cell_volume                     1415.1(2)
_computing_cell_refinement       'SAINT V8.18C (?, 2016)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT V8.18C (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293.15
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.760
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0227
_diffrn_reflns_av_unetI/netI     0.0283
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.760
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            16266
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.760
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.335
_diffrn_reflns_theta_min         1.849
_diffrn_source_current           30.0
_diffrn_source_power             1.35
_diffrn_source_voltage           45.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.704
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.4205
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'clear dark violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.741
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             727
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.352
_refine_diff_density_min         -0.752
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     404
_refine_ls_number_reflns         7064
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0381
_refine_ls_R_factor_gt           0.0294
_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^)+(0.0389P)^2^+0.3385P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0731
_refine_ls_wR_factor_ref         0.0777
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5844
_reflns_number_total             7064
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj00866h2.cif
_cod_data_source_block           ds250113_0m
_cod_depositor_comments
'Adding full bibliography for 7060691--7060692.cif.'
_cod_database_code               7060692
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.772
_shelx_estimated_absorpt_t_min   0.629
_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. Others
 Sof(Sb6A)=1-FVAR(1)
 Sof(Sb6)=FVAR(1)
 Sof(F0AB)=Sof(F4A)=1-FVAR(2)
 Sof(F4)=FVAR(2)
 Sof(F2A)=Sof(F5A)=1-FVAR(3)
 Sof(F2)=Sof(F5)=FVAR(3)
 Sof(F7)=1-FVAR(4)
 Sof(F0AA)=Sof(F6)=FVAR(4)
3.a Ternary CH refined with riding coordinates:
 C00K(H00K), C00S(H00S)
3.b Secondary CH2 refined with riding coordinates:
 C00I(H00c,H00g), C00T(H00h,H00i)
3.c Aromatic/amide H refined with riding coordinates:
 C009(H009), C00A(H00A), C00B(H00B), C00D(H00D), C00E(H00E), C00F(H00F),
 C00J(H00J), C00L(H00L), C00N(H00N), C00O(H00O), C00P(H00P), C00Q(H00Q),
 C00U(H00U), C00W(H00W), C00Y(H00z)
3.d Idealised Me refined as rotating group:
 C00V(H00m,H00r,H00t), C00X(H00v,H00x,H00y)
;
_shelx_res_checksum              70313
_olex2_submission_special_instructions 'No special instructions were received'