Never a dull moment with praseodymium metal
Guo, Zhifang; Deacon, Glen B.; Junk, Peter Courtney; Dalton Transactions  (2023) –; doi:10.1039/D3DT00534H

data_7712674
_publ_section_title
;
 Never a dull moment with praseodymium metal
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00534H
_journal_year                    2023
_chemical_formula_moiety         'C62 H70 Bi2 F10 N4'
_chemical_formula_sum            'C62 H70 Bi2 F10 N4'
_chemical_formula_weight         1479.18
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-02-19
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-02-19 deposited with the CCDC.	2023-03-24 downloaded from the CCDC.
;
_cell_angle_alpha                105.9880(9)
_cell_angle_beta                 106.5627(10)
_cell_angle_gamma                102.5770(9)
_cell_formula_units_Z            1
_cell_length_a                   11.32528(13)
_cell_length_b                   12.25378(12)
_cell_length_c                   12.54848(12)
_cell_measurement_reflns_used    31253
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      33.8980
_cell_measurement_theta_min      3.4190
_cell_volume                     1519.42(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (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      123.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.884
_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    -42.00  38.00   0.50    6.23    --   12.96 -82.00 -78.00  160
  2  \w    -23.00  46.00   0.50    6.23    --   12.96 -99.00  30.00  138
  3  \w    -42.00  11.00   0.50    6.23    --  -13.74 -82.00 -78.00  106
  4  \w    -60.00  25.00   0.50    6.23    --   12.96 -37.00-120.00  170
  5  \w     -2.00  85.00   0.50    6.23    --   12.96  57.00-180.00  174
  6  \w     41.00  86.00   0.50    6.23    --   12.96 178.00-120.00   90
  7  \w     41.00  86.00   0.50    6.23    --   12.96 178.00 -30.00   90
  8  \w     41.00  86.00   0.50    6.23    --   12.96 178.00  60.00   90
  9  \w     -2.00  85.00   0.50    6.23    --   12.96  57.00  60.00  174
 10  \w     41.00  86.00   0.50    6.23    --   12.96 178.00-150.00   90
 11  \w    -29.00   1.00   0.50    6.23    --  -13.74  57.00   0.00   60
 12  \w    -39.00  21.00   0.50    6.23    --  -13.74  82.00  43.00  120
 13  \w    -85.00   1.00   0.50    6.23    --  -13.74 -57.00 -60.00  172
 14  \w    -85.00   9.00   0.50    6.23    --  -13.74 -77.00-120.00  188
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0567674000
_diffrn_orient_matrix_UB_12      0.0213859000
_diffrn_orient_matrix_UB_13      0.0522067000
_diffrn_orient_matrix_UB_21      0.0096474000
_diffrn_orient_matrix_UB_22      -0.0566091000
_diffrn_orient_matrix_UB_23      -0.0167690000
_diffrn_orient_matrix_UB_31      0.0380278000
_diffrn_orient_matrix_UB_32      0.0195382000
_diffrn_orient_matrix_UB_33      -0.0314849000
_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  0.0399
_diffrn_reflns_av_unetI/netI     0.0341
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.884
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            49963
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.884
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.886
_diffrn_reflns_theta_min         3.427
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.854
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68601
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
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    1.617
_exptl_crystal_description       block
_exptl_crystal_F_000             726
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.146
_refine_diff_density_min         -1.049
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     364
_refine_ls_number_reflns         10875
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0297
_refine_ls_R_factor_gt           0.0242
_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^)+(0.0306P)^2^+0.1373P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0557
_refine_ls_wR_factor_ref         0.0570
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9832
_reflns_number_total             10875
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00534h2.cif
_cod_data_source_block           exp_1218
_cod_database_code               7712674
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         PrCHNOF
_shelx_estimated_absorpt_t_max   0.592
_shelx_estimated_absorpt_t_min   0.273
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H18A,H18B,H18C} of C18, {H12A,H12B,H12C} of C12, {H25A,
  H25B,H25C} of C25, {H11A,H11B,H11C} of C11
 At 1.5 times of:
  {H2A,H2B,H2C} of C2, {H1A,H1B,H1C} of C1, {H17A,H17B,H17C} of C17, {H24A,
  H24B,H24C} of C24
2. Rigid bond restraints
 C20, C19
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C25, C23
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C20, C21
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
3. Uiso/Uaniso restraints and constraints
C20 \\sim C19: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
C25 \\sim C23: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
C20 \\sim C21: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
4.a Ternary CH refined with riding coordinates:
 C10(H10), C16(H16), C23(H23), C3(H3)
4.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C6(H6), C5(H5), C21(H21), C19(H19), C20(H20)
4.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C1(H1A,H1B,H1C), C24(H24A,H24B,H24C), C17(H17A,H17B,H17C),
 C18(H18A,H18B,H18C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C25(H25A,H25B,
 H25C)
;
_shelx_res_checksum              90188
_shelx_hkl_checksum              75885
_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 1.455
_oxdiff_exptl_absorpt_empirical_full_min 0.809