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_7060691
_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 Cl N P Pd, C2.5 H3.5'
_chemical_formula_sum            'C29.5 H30.5 Cl N P Pd'
_chemical_formula_weight         571.87
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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                90
_cell_angle_beta                 110.1600(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.378(3)
_cell_length_b                   10.2854(12)
_cell_length_c                   21.374(3)
_cell_measurement_reflns_used    5749
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.26
_cell_measurement_theta_min      2.51
_cell_volume                     5237.3(11)
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.907
_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  0.0418
_diffrn_reflns_av_unetI/netI     0.0399
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.907
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            20251
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.907
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.416
_diffrn_reflns_theta_min         1.710
_diffrn_source_current           30.0
_diffrn_source_power             1.35
_diffrn_source_voltage           45.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.890
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6392
_exptl_crystal_colour            'clear dark blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.451
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2340
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.426
_refine_diff_density_min         -0.570
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         5421
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0531
_refine_ls_R_factor_gt           0.0358
_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^)+(0.0484P)^2^+4.0107P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0862
_refine_ls_wR_factor_ref         0.0960
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4213
_reflns_number_total             5421
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj00866h2.cif
_cod_data_source_block           ds010214r2_0m
_cod_depositor_comments
'Adding full bibliography for 7060691--7060692.cif.'
_cod_original_formula_sum        'C29.50 H30.50 Cl N P Pd'
_cod_database_code               7060691
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.886
_shelx_estimated_absorpt_t_min   0.789
_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. Restrained distances
 C00Q-C00R \\sim C3-C1
 with sigma of 0.04
 C00Q-C00X \\sim C3-C2
 with sigma of 0.02
 C00R-C00X \\sim C1-C2
 with sigma of 0.02
 Pd01-C00X \\sim Pd01-C2
 with sigma of 0.04
 Pd01-C00Q \\sim Pd01-C3
 with sigma of 0.04
 Pd01-C00R \\sim Pd01-C1
 with sigma of 0.04
3. Others
 Sof(C1)=Sof(H1a)=Sof(H1b)=Sof(C2)=Sof(H2)=Sof(C3)=Sof(H3a)=Sof(H3b)=1-FVAR(1)
 Sof(C00Q)=Sof(H00i)=Sof(H00l)=Sof(C00R)=Sof(H00q)=Sof(H00r)=Sof(C00X)=
 Sof(H00z)=FVAR(1)
 Fixed Sof: H00(0.5) H(0.5) Ha(0.5)
4.a Ternary CH refined with riding coordinates:
 C00X(H00z), C2(H2)
4.b Secondary CH2 refined with riding coordinates:
 C00Q(H00i,H00l), C00R(H00q,H00r), C00Y(H1,Hb), C1(H1a,H1b), C3(H3a,H3b)
4.c Aromatic/amide H refined with riding coordinates:
 C009(H009), C00A(H00A), C00B(H00B), C00C(H00C), C00D(H00D), C00E(H00E),
 C00F(H00F), C00G(H00G), C00H(H00H), C00J(H00J), C00K(H00K), C00M(H00M),
 C00N(H00N), C00O(H00O), C00P(H00P), C00U(H00v)
4.d Idealised Me refined as rotating group:
 C00S(H00,H,Ha), C00T(H00s,H00t,H00u), C00V(H00w,H00x,H00y)
;
_shelx_res_checksum              95801
_olex2_submission_special_instructions 'No special instructions were received'