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

data_7712673
_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         'C60 H44 Bi2 N8, C4 H8 O2'
_chemical_formula_sum            'C64 H52 Bi2 N8 O2'
_chemical_formula_weight         1383.09
_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
_audit_creation_date             2023-01-19
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
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2023-02-19 deposited with the CCDC.	2023-03-24 downloaded from the CCDC.
;
_cell_angle_alpha                117.21(3)
_cell_angle_beta                 90.85(3)
_cell_angle_gamma                101.57(3)
_cell_formula_units_Z            1
_cell_length_a                   9.7300(19)
_cell_length_b                   12.096(2)
_cell_length_c                   12.680(3)
_cell_measurement_reflns_used    792
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29
_cell_measurement_theta_min      2
_cell_volume                     1290.5(6)
_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    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0771
_diffrn_reflns_av_unetI/netI     0.0404
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            23882
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.820
_diffrn_source                   'MX1 Beamline Australian Synchrotron'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.865
_exptl_absorpt_correction_T_max  0.918
_exptl_absorpt_correction_T_min  0.627
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XDS(Kabsch, 1993)'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.780
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             674
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.071
_refine_diff_density_min         -2.011
_refine_diff_density_rms         0.177
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     363
_refine_ls_number_reflns         4548
_refine_ls_number_restraints     52
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0375
_refine_ls_R_factor_gt           0.0346
_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^)+(0.0557P)^2^+3.6203P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0894
_refine_ls_wR_factor_ref         0.0909
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4271
_reflns_number_total             4548
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00534h2.cif
_cod_data_source_block           1
_cod_database_code               7712673
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.610
_shelx_estimated_absorpt_t_min   0.547
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H5(0.033) H20(0.033) H8(0.029) H23(0.028) H16(0.036) H4(0.036)
 H26(0.036) H30(0.028) H1(0.034) H2(0.038) H19(0.037) H15(0.043) H27(0.038)
 H17(0.042) H18(0.041) H3(0.042) H28(0.036) H14(0.05) H29(0.035) H13(0.062)
 H13A(0.062) H11(0.075) H11A(0.075) H12(0.062) H31B(0.079) H31A(0.079)
 H31D(0.079) H31C(0.079) H32A(0.134) H32B(0.134) H32C(0.134) H32D(0.134)
 H12A(0.062)
 Fixed X: H5(0.184741) H20(0.91799) H8(0.137185) H23(0.933507) H16(0.508949)
 H4(0.147169) H26(0.719404) H30(1.087904) H1(0.20649) H2(0.181608)
 H19(0.877222) H15(0.091437) H27(0.83652) H17(0.469271) H18(0.655085)
 H3(0.148344) H28(1.076456) H14(0.109881) H29(1.201383) H13(0.300276)
 H13A(0.319155) H11(0.459091) H11A(0.477438) H12(0.511556) H31B(0.658008)
 H31A(0.561047) H31D(0.633721) H31C(0.476014) H32A(0.420735) H32B(0.584193)
 H32C(0.490044) H32D(0.592685) H12A(0.446608)
 Fixed Y: H5(0.496425) H20(0.825626) H8(0.531237) H23(0.772974) H16(0.677603)
 H4(0.476474) H26(0.874084) H30(0.876914) H1(0.876622) H2(0.858423)
 H19(0.733579) H15(0.482489) H27(0.885033) H17(0.587451) H18(0.61076)
 H3(0.656126) H28(0.888132) H14(0.383197) H29(0.883897) H13(0.461514)
 H13A(0.438729) H11(0.735463) H11A(0.712327) H12(0.57841) H31B(0.995186)
 H31A(0.883721) H31D(0.912156) H31C(0.926429) H32A(0.813685) H32B(0.816936)
 H32C(0.777094) H32D(0.888836) H12A(0.658421)
 Fixed Z: H5(0.483753) H20(0.697062) H8(0.303009) H23(0.452436) H16(0.550733)
 H4(0.657993) H26(0.194941) H30(0.350254) H1(0.672188) H2(0.848316)
 H19(0.823148) H15(0.093079) H27(0.039431) H17(0.679042) H18(0.81196)
 H3(0.838642) H28(0.037336) H14(-0.110412) H29(0.192368) H13(-0.184228) H13A(-
 0.179264) H11(0.146784) H11A(0.151063) H12(-0.043857) H31B(0.943447)
 H31A(0.827213) H31D(0.862997) H31C(0.853547) H32A(0.945706) H32B(0.972072)
 H32C(0.923634) H32D(1.040934) H12A(-0.058892)
;
_shelx_res_checksum              42089
_shelx_hkl_checksum              74325
_olex2_submission_special_instructions 'No special instructions were received'