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

data_7712675
_publ_section_title
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 Never a dull moment with praseodymium metal
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_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00534H
_journal_year                    2023
_chemical_formula_moiety         'C56 H70 Bi F5 N4'
_chemical_formula_sum            'C56 H70 Bi F5 N4'
_chemical_formula_weight         1103.14
_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             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                73.17(3)
_cell_angle_beta                 77.93(3)
_cell_angle_gamma                70.19(3)
_cell_formula_units_Z            2
_cell_length_a                   10.980(2)
_cell_length_b                   12.580(3)
_cell_length_c                   21.130(4)
_cell_measurement_reflns_used    9171
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2
_cell_volume                     2608.3(11)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_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_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'Phi Scan'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_source         'MX1 Beamline Australian Synchrotron'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0317
_diffrn_reflns_av_unetI/netI     0.0225
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            45146
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.025
_diffrn_reflns_theta_max         25.025
_diffrn_reflns_theta_min         1.015
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.437
_exptl_absorpt_correction_T_max  0.7
_exptl_absorpt_correction_T_min  0.5
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XDS(Kabsch, 1993)'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.405
_exptl_crystal_description       prism
_exptl_crystal_F_000             1124
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.225
_refine_diff_density_min         -1.039
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     631
_refine_ls_number_reflns         9171
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0235
_refine_ls_R_factor_gt           0.0214
_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^)+(0.0305P)^2^+1.2918P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0511
_refine_ls_wR_factor_ref         0.0520
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8670
_reflns_number_total             9171
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00534h2.cif
_cod_data_source_block           p-1
_cod_database_code               7712675
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.875
_shelx_estimated_absorpt_t_min   0.725
_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. Uiso/Uaniso restraints and constraints
C49A \\sim C49: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.01 within 2A
C20 \\sim C21 \\sim C22: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.01 within 2A
3. Others
 Fixed Sof: H48(0.6) H48A(0.4) C50(0.6) H50A(0.6) H50B(0.6) H50C(0.6) C49(0.8)
 H49A(0.9) H49B(0.9) H49C(0.9) C50A(0.4) H50D(0.4) H50E(0.4) H50F(0.4)
 C49A(0.2) H49D(0.1) H49E(0.1) H49F(0.1)
4.a Ternary CH refined with riding coordinates:
 C2(H2), C10(H10), C20(H20), C45(H45), C35(H35), C28(H28), C23(H23), C48(H48),
 C48(H48A)
4.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C38(H38), C16(H16), C31(H31), C5(H5), C32(H32), C30(H30), C7(H7),
 C6(H6), C18(H18), C17(H17), C43(H43), C41(H41), C42(H42)
4.c Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C26(H26A,H26B,
 H26C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C46(H46A,H46B,H46C), C27(H27A,
 H27B,H27C), C1(H1A,H1B,H1C), C25(H25A,H25B,H25C), C47(H47A,H47B,H47C),
 C24(H24A,H24B,H24C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C50(H50A,H50B,
 H50C), C49(H49A,H49B,H49C), C50A(H50D,H50E,H50F), C49A(H49D,H49E,H49F)
;
_shelx_res_checksum              31306
_shelx_hkl_checksum              93160
_olex2_submission_special_instructions 'No special instructions were received'