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

data_7712677
_publ_section_title
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 Never a dull moment with praseodymium metal
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00534H
_journal_year                    2023
_chemical_formula_moiety         'C54 H78 F N4 O Pr, C7 H8'
_chemical_formula_sum            'C61 H86 F N4 O Pr'
_chemical_formula_weight         1051.24
_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   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                90
_cell_angle_beta                 92.9560(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.0787(2)
_cell_length_b                   13.8725(2)
_cell_length_c                   33.8375(5)
_cell_measurement_reflns_used    40121
_cell_measurement_temperature    123.00(12)
_cell_measurement_theta_max      33.4930
_cell_measurement_theta_min      3.3470
_cell_volume                     5662.33(15)
_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  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.00(12)
_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 0.889
_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    -23.00  46.00   0.50   51.75    --   12.02 -99.00  90.00  138
  2  \w     26.00  75.00   0.50   51.75    --   12.02-151.00   8.00   98
  3  \w     11.00  58.00   0.50   51.75    --   12.02-122.00 169.00   94
  4  \w    -23.00  46.00   0.50   51.75    --   12.02 -99.00 -60.00  138
  5  \w     38.00  85.00   0.50   51.75    --   12.02-178.00-180.00   94
  6  \w    -84.00   2.00   0.50   51.75    --  -12.80 -57.00-180.00  172
  7  \w    -84.00 -59.00   0.50   51.75    --  -12.80 -77.00 -30.00   50
  8  \w    -84.00   2.00   0.50   51.75    --  -12.80 -57.00 120.00  172
;
_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      0.0056691000
_diffrn_orient_matrix_UB_12      0.0437206000
_diffrn_orient_matrix_UB_13      0.0107720000
_diffrn_orient_matrix_UB_21      0.0021507000
_diffrn_orient_matrix_UB_22      0.0259990000
_diffrn_orient_matrix_UB_23      -0.0180038000
_diffrn_orient_matrix_UB_31      -0.0584840000
_diffrn_orient_matrix_UB_32      0.0051561000
_diffrn_orient_matrix_UB_33      -0.0007006000
_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  0.0458
_diffrn_reflns_av_unetI/netI     0.0447
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.889
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            95583
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.889
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.550
_diffrn_reflns_theta_min         3.353
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.905
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75160
_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    1.233
_exptl_crystal_description       block
_exptl_crystal_F_000             2224
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.061
_refine_diff_density_min         -0.790
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     648
_refine_ls_number_reflns         19825
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0530
_refine_ls_R_factor_gt           0.0328
_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^)+(0.0368P)^2^+0.9759P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0722
_refine_ls_wR_factor_ref         0.0772
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15222
_reflns_number_total             19825
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00534h2.cif
_cod_data_source_block           exp_1249
_cod_database_code               7712677
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         PrCHNOF
_shelx_estimated_absorpt_t_max   0.915
_shelx_estimated_absorpt_t_min   0.840
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     29.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: H48(0.4) H48A(0.6) C49(0.4) H49A(0.4) H49B(0.4) H49C(0.4) C62(0.6)
 H62A(0.6) H62B(0.6) H62C(0.6)
3.a Ternary CH refined with riding coordinates:
 C45(H45), C48(H48), C48(H48A), C2(H2), C27(H27), C35(H35), C16(H16), C23(H23),
  C10(H10)
3.b Secondary CH2 refined with riding coordinates:
 C54(H54A,H54B), C51(H51A,H51B), C52(H52A,H52B), C53(H53A,H53B)
3.c Aromatic/amide H refined with riding coordinates:
 C41(H41), C43(H43), C42(H42), C32(H32), C30(H30), C31(H31), C19(H19), C5(H5),
 C7(H7), C21(H21), C6(H6), C20(H20), C57(H57), C58(H58), C60(H60), C61(H61),
 C59(H59)
3.d Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C1(H1A,H1B,H1C), C47(H47A,H47B,H47C), C12(H12A,H12B,
 H12C), C18(H18A,H18B,H18C), C17(H17A,H17B,H17C), C3(H3A,H3B,H3C), C26(H26A,
 H26B,H26C), C46(H46A,H46B,H46C), C37(H37A,H37B,H37C), C11(H11A,H11B,H11C),
 C50(H50A,H50B,H50C), C25(H25A,H25B,H25C), C24(H24A,H24B,H24C), C36(H36A,H36B,
 H36C), C49(H49A,H49B,H49C), C55(H55A,H55B,H55C), C62(H62A,H62B,H62C)
;
_shelx_res_checksum              40722
_shelx_hkl_checksum              69618
_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 1.599
_oxdiff_exptl_absorpt_empirical_full_min 0.835