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

data_7718634
_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 N O2 P Re'
_chemical_formula_sum            'C16 H23 N O2 P Re'
_chemical_formula_weight         478.52
_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             2024-11-20
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2025-02-13 deposited with the CCDC.	2025-04-30 downloaded from the CCDC.
;
_cell_angle_alpha                91.653(4)
_cell_angle_beta                 94.080(4)
_cell_angle_gamma                93.172(5)
_cell_formula_units_Z            2
_cell_length_a                   6.5007(4)
_cell_length_b                   10.3978(6)
_cell_length_c                   12.9967(6)
_cell_measurement_reflns_used    4211
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      27.5160
_cell_measurement_theta_min      3.8340
_cell_volume                     874.44(8)
_computing_cell_refinement       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_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                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1872
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.791
_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    -37.00  37.00   1.00    1.00    --   -9.26  77.00  30.00   74
  2  \w    -34.00  16.00   1.00    1.00    --   -9.26 -77.00 -90.00   50
  3  \w    -37.00  42.00   1.00    1.00    --    9.42 -77.00 150.00   79
  4  \w    -19.00  82.00   1.00    1.00    --    9.42  57.00 -60.00  101
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0819236000
_diffrn_orient_matrix_UB_12      0.0365683000
_diffrn_orient_matrix_UB_13      -0.0198238000
_diffrn_orient_matrix_UB_21      0.0661856000
_diffrn_orient_matrix_UB_22      0.0567277000
_diffrn_orient_matrix_UB_23      0.0052500000
_diffrn_orient_matrix_UB_31      0.0302279000
_diffrn_orient_matrix_UB_32      -0.0108409000
_diffrn_orient_matrix_UB_33      -0.0507576000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0476
_diffrn_reflns_av_unetI/netI     0.0799
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.791
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7683
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.791
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.273
_diffrn_reflns_theta_min         3.414
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    7.043
_exptl_absorpt_correction_T_max  0.367
_exptl_absorpt_correction_T_min  0.182
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.82a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_density_diffrn    1.817
_exptl_crystal_description       block
_exptl_crystal_F_000             464
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH2Cl2/hexane'
_exptl_crystal_size_max          0.341
_exptl_crystal_size_mid          0.233
_exptl_crystal_size_min          0.195
_refine_diff_density_max         1.349
_refine_diff_density_min         -2.131
_refine_diff_density_rms         0.232
_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     190
_refine_ls_number_reflns         3780
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0404
_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^)+(0.0280P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0751
_refine_ls_wR_factor_ref         0.0824
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3340
_reflns_number_total             3780
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00992h2.cif
_cod_data_source_block           rmk_381_b_2_scale2
_cod_depositor_comments
'Adding full bibliography for 7718628--7718640.cif.'
_cod_database_code               7718634
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C16H23N1O2P1Re1
_chemical_oxdiff_usercomment     'hexane at -30 deg '
_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. Uiso/Uaniso restraints and constraints
Uanis(C2) = Uanis(O2)
3.a Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C16(H16), C15(H15), C14(H14)
3.b Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C7(H7A,H7B,H7C), C9(H9A,H9B,H9C), C6(H6A,H6B,H6C),
 C5(H5A,H5B,H5C), C11(H11A,H11B,H11C)
;
_shelx_res_checksum              21695
_shelx_hkl_checksum              33278
_ins_header
;
TITL RMK_381_B_2_scale2 in P1 
REM P1 (#1 in standard setting)
CELL 0.71073   6.500669  10.397827  12.996701  91.6526  94.0802  93.1718
ZERR    2.00   0.000358   0.000600   0.000634   0.0043   0.0042   0.0046
LATT -1
SFAC C H N O P Re
UNIT 32.00 46.00 2.00 4.00 2.00 2.00
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 1.178
_oxdiff_exptl_absorpt_empirical_full_min 0.762