Alkynyltellurolato ligands including a solvatochromic rhenium(i) complex
Burt, Liam K.; Kirk, Ryan M.; Hill, Anthony F.; Chemical Communications 61 (2025) 6150–6153; doi:10.1039/D5CC00770D

data_7134336
_publ_section_title
;
 Alkynyltellurolato ligands including a solvatochromic rhenium(i) complex
;
_journal_issue                   33
_journal_name_full               'Chemical Communications'
_journal_page_first              6150
_journal_page_last               6153
_journal_paper_doi               10.1039/D5CC00770D
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'C32 H25 Fe O P Te'
_chemical_formula_sum            'C32 H25 Fe O P Te'
_chemical_formula_weight         639.94
_chemical_properties_physical    Air-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-01-11
_audit_creation_method
;
Olex2 1.2
(compiled Aug 10 2017 17:28:52 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2025-02-11 deposited with the CCDC.	2025-03-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.031(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.6985(2)
_cell_length_b                   19.2903(5)
_cell_length_c                   17.9591(5)
_cell_measurement_reflns_used    12406
_cell_measurement_temperature    149.97(18)
_cell_measurement_theta_max      29.4270
_cell_measurement_theta_min      3.8590
_cell_volume                     2665.37(12)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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_environment      N~2~
_diffrn_ambient_temperature      149.97(18)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3744
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.886
_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    -83.00  17.00   1.00   21.00    --  -11.22 -57.00-150.00  100
  2  \w    -87.00  21.00   1.00   21.00    --  -11.22 -77.00  90.00  108
  3  \w    -39.00  62.00   1.00   21.00    --  -11.22  57.00   0.00  101
  4  \w    -83.00 -58.00   1.00   21.00    --  -11.22 -57.00 -30.00   25
  5  \w    -20.00  52.00   1.00   21.00    --   11.46 -99.00 150.00   72
  6  \w     35.00 100.00   1.00   21.00    --   11.46 178.00 -30.00   65
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, Atlas'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0162207000
_diffrn_orient_matrix_UB_12      -0.0347247000
_diffrn_orient_matrix_UB_13      0.0111907000
_diffrn_orient_matrix_UB_21      -0.0033623000
_diffrn_orient_matrix_UB_22      -0.0105731000
_diffrn_orient_matrix_UB_23      -0.0378645000
_diffrn_orient_matrix_UB_31      0.0906692000
_diffrn_orient_matrix_UB_32      0.0058490000
_diffrn_orient_matrix_UB_33      -0.0019757000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0374
_diffrn_reflns_av_unetI/netI     0.0326
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.886
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            35878
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.886
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.001
_diffrn_reflns_theta_min         3.366
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.722
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73367
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.595
_exptl_crystal_description       plate
_exptl_crystal_F_000             1272
_exptl_crystal_recrystallization_method
'Crystals grown from vapor-vapor diffusion of n-pentane into DCM solution.'
_exptl_crystal_size_max          0.296
_exptl_crystal_size_mid          0.212
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.413
_refine_diff_density_min         -0.562
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         6886
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0446
_refine_ls_R_factor_gt           0.0315
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0216P)^2^+3.8858P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0629
_refine_ls_wR_factor_ref         0.0706
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5718
_reflns_number_total             6886
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc00770d2.cif
_cod_data_source_block           lb-1-40_scale
_cod_depositor_comments
'Adding full bibliography for 7134336--7134337.cif.'
_cod_database_code               7134336
_shelx_shelxl_version_number     2016/4
_chemical_oxdiff_formula         'C32 H25 Fe1 O1 P1 Te1'
_chemical_oxdiff_usercomment     'Green Xtal from DCM/Pent Vap'
_reflns_odcompleteness_completeness 99.72
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C26(H26), C16(H16), C22(H22), C3(H3), C4(H4), C2(H2), C25(H25), C17(H17),
 C23(H23), C20(H20), C5(H5), C18(H18), C19(H19), C6(H6), C30(H30), C32(H32),
 C24(H24), C29(H29), C28(H28), C10(H10), C31(H31), C11(H11), C14(H14), C13(H13),
  C12(H12)
;
_shelx_res_checksum              52349
_shelx_hkl_checksum              73831
_ins_header
;
TITL LB-1-40_scale in P2(1)/n 
REM P2(1)/n (#14 in standard setting)
CELL 0.71073   7.698522  19.290303  17.959094  90.0000  92.0311  90.0000
ZERR    4.00   0.000236   0.000527   0.000504   0.0000   0.0027   0.0000
LATT  1
SYMM -x+1/2, y+1/2,-z+1/2 
SFAC C H O P Fe Te
UNIT 128.00 100.00 4.00 4.00 4.00 4.00
TREF
HKLF 4
END
;
_olex2_submission_original_sample_id LB-1-40
_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 1.280
_oxdiff_exptl_absorpt_empirical_full_min 0.727