Pnictogen-functionalised isocyanide ligands.
Kirk, Ryan M.; Hill, Anthony F.; Dalton transactions (Cambridge, England : 2003) 54 (2025) 8881–8887; doi:10.1039/d5dt00992h

data_7718639
_publ_section_title
;
 Pnictogen-functionalised isocyanide ligands.
;
_journal_issue                   22
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8881
_journal_page_last               8887
_journal_paper_doi               10.1039/d5dt00992h
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C16 H23 Mn N O2 P'
_chemical_formula_sum            'C16 H23 Mn N O2 P'
_chemical_formula_weight         347.26
_chemical_properties_physical    Air-sensitive
_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             2024-11-20
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-11-20 deposited with the CCDC.	2025-04-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.390(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.3531(6)
_cell_length_b                   6.3326(3)
_cell_length_c                   26.3915(13)
_cell_measurement_reflns_used    4572
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      26.9180
_cell_measurement_theta_min      2.5430
_cell_volume                     1729.77(16)
_computing_cell_refinement       'CrysAlisPro 1.171.42.85a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.85a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.85a (Rigaku OD, 2023)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.795
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -16.00  16.00   0.50    2.00    --   -4.70  29.00-126.00   64
  2  \w    -68.00   4.00   0.50    2.00    --   -4.70 -29.00  71.00  144
  3  \w    -24.00  35.00   0.50    2.00    --    1.66 -99.00-180.00  118
  4  \w     -9.00  75.00   0.50    2.00    --    1.66  38.00 -30.00  168
  5  \w    -72.00  16.00   0.50    2.00    --    1.66 -38.00-180.00  176
  6  \w    -51.00 -26.00   0.50    2.00    --    1.66 -38.00  30.00   50
  7  \w     -6.00  26.00   0.50    2.00    --   -4.70 -99.00 -60.00   64
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0334727000
_diffrn_orient_matrix_UB_12      0.0899693000
_diffrn_orient_matrix_UB_13      0.0088756000
_diffrn_orient_matrix_UB_21      -0.0597294000
_diffrn_orient_matrix_UB_22      -0.0522605000
_diffrn_orient_matrix_UB_23      -0.0045701000
_diffrn_orient_matrix_UB_31      0.0026814000
_diffrn_orient_matrix_UB_32      -0.0415143000
_diffrn_orient_matrix_UB_33      0.0249612000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0881
_diffrn_reflns_av_unetI/netI     0.0641
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.795
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            22496
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.795
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.888
_diffrn_reflns_theta_min         2.472
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.859
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71361
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.85a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_description       prism
_exptl_crystal_F_000             728
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: hexane'
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.507
_refine_diff_density_min         -0.344
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         4339
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0676
_refine_ls_R_factor_gt           0.0444
_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^)+(0.0313P)^2^+1.1099P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0881
_refine_ls_wR_factor_ref         0.1017
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3226
_reflns_number_total             4339
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00992h2.cif
_cod_data_source_block           rmk_377_b_scale
_cod_depositor_comments
'Adding full bibliography for 7718628--7718640.cif.'
_cod_database_code               7718639
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C16H23Mn1N1O2P1
_chemical_oxdiff_usercomment     'hexane evap at -30 '
_shelx_estimated_absorpt_t_max   0.927
_shelx_estimated_absorpt_t_min   0.747
_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:
 C15(H15), C16(H16), C14(H14), C12(H12), C13(H13)
2.b Idealised Me refined as rotating group:
 C11(H11a,H11b,H11c), C9(H9a,H9b,H9c), C7(H7a,H7b,H7c), C10(H10a,H10b,H10c),
 C5(H5a,H5b,H5c), C6(H6a,H6b,H6c)
;
_shelx_res_checksum              40553
_shelx_hkl_checksum              15957
_ins_header
;
TITL RMK_377_B_scale in P2(1)/c 
REM P2(1)/c (#14 in standard setting)
CELL 0.71073  10.353067   6.332631  26.391526  90.0000  91.3904  90.0000
ZERR    4.00   0.000567   0.000342   0.001268   0.0000   0.0046   0.0000
LATT  1
SYMM -x, y+1/2,-z+1/2 
SFAC C H N O P Mn
UNIT 64.00 92.00 4.00 8.00 4.00 4.00
REM  CrysAlisPro recorded range (K): Min=150.0; max=150.0; aver:150.0
TEMP -123
SIZE 0.09 0.23 0.36
TREF
HKLF 4
END
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.505
_oxdiff_exptl_absorpt_empirical_full_min 0.734