(Isocyano group)⋯lone pair interactions involving coordinated isocyanides: experimental, theoretical and CSD studies
Mikherdov, Alexander S.; Katkova, Svetlana A.; Novikov, Alexander S.; Efremova, Mariia M.; Reutskaya, Elena Yu.; Kinzhalov, Mikhail A.; CrystEngComm 22 (2020) 1154–1159; doi:10.1039/C9CE01741K

data_7239762
_publ_section_title
;
 (Isocyano group)&#x22EF;lone pair interactions involving coordinated
 isocyanides: experimental, theoretical and CSD studies
;
_journal_issue                   7
_journal_name_full               CrystEngComm
_journal_page_first              1154
_journal_page_last               1159
_journal_paper_doi               10.1039/C9CE01741K
_journal_volume                  22
_journal_year                    2020
_chemical_formula_moiety         'C24 H25 Cl I N5 Pd'
_chemical_formula_sum            'C24 H25 Cl I N5 Pd'
_chemical_formula_weight         652.24
_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     dual
_audit_creation_date             2019-03-15
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-04-10 deposited with the CCDC.	2020-01-16 downloaded from the CCDC.
;
_cell_angle_alpha                68.122(8)
_cell_angle_beta                 86.872(7)
_cell_angle_gamma                80.728(6)
_cell_formula_units_Z            2
_cell_length_a                   8.8377(6)
_cell_length_b                   11.5913(9)
_cell_length_c                   12.6874(11)
_cell_measurement_reflns_used    4202
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      30.5550
_cell_measurement_theta_min      3.0190
_cell_volume                     1190.32(18)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_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      100.01(10)
_diffrn_detector_area_resol_mean 16.2096
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.865
_diffrn_measurement_details
;
  1 omega  -95.00  -43.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      -22.4031  178.0000 -180.0000 52

  2 omega    8.00   65.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -       23.3406  -99.0000    0.0000 57

  3 omega    8.00   76.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -       23.3406 -117.0000 -137.0000 68

  4 omega    3.00   96.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -       23.3406   19.0000  150.0000 93

  5 omega   20.00   64.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -       23.3406  -99.0000  120.0000 44

  6 omega  -50.00   57.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -       23.3406    0.0000  -60.0000 107
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0444071000
_diffrn_orient_matrix_UB_12      -0.0584759000
_diffrn_orient_matrix_UB_13      0.0048413000
_diffrn_orient_matrix_UB_21      0.0064269000
_diffrn_orient_matrix_UB_22      -0.0162982000
_diffrn_orient_matrix_UB_23      0.0594647000
_diffrn_orient_matrix_UB_31      -0.0678233000
_diffrn_orient_matrix_UB_32      -0.0276770000
_diffrn_orient_matrix_UB_33      0.0083734000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_av_unetI/netI     0.0542
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.865
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11601
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.865
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.086
_diffrn_reflns_theta_min         2.787
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.211
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88016
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.820
_exptl_crystal_description       prism
_exptl_crystal_F_000             640
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.687
_refine_diff_density_min         -0.777
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     295
_refine_ls_number_reflns         6611
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0450
_refine_ls_R_factor_gt           0.0322
_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^)+(0.0218P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0630
_refine_ls_wR_factor_ref         0.0696
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5393
_reflns_number_total             6611
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce01741k8.cif
_cod_data_source_block           3
_cod_depositor_comments
;Adding full bibliography for 7239762.cif.

 Adding full bibliography for 7239762.cif.
;
_cod_original_cell_volume        1190.32(17)
_cod_database_code               7239762
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Pd2 C43 N12 Cl2 I'
_shelx_estimated_absorpt_t_max   0.809
_shelx_estimated_absorpt_t_min   0.809
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.51
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N2(H2), C4(H4), C5(H5), C13(H13), C14(H14), C6(H6), C15(H15)
2.b Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C8(H8A,H8B,H8C), C18(H18A,H18B,H18C), C9(H9A,H9B,H9C),
 C17(H17A,H17B,H17C), C23(H23A,H23B,H23C)
;
_olex2_submission_special_instructions 'No special instructions were received'