A tetravalent praseodymium complex with field-induced slow magnetic relaxation.
Xue, Tianjiao; Ding, You-Song; Zheng, Zhiping; Dalton transactions (Cambridge, England : 2003) 53 (2024) 5779–5783; doi:10.1039/d4dt00052h

data_7715413
_publ_section_title
;
 A tetravalent praseodymium complex with field-induced slow magnetic
 relaxation.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5779
_journal_page_last               5783
_journal_paper_doi               10.1039/d4dt00052h
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C66 H69 O6 Pr Si3, C4 H8 O'
_chemical_formula_sum            'C70 H77 O7 Pr Si3'
_chemical_formula_weight         1255.49
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2024-01-02
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-01-05 deposited with the CCDC.	2024-03-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 115.0839(13)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.6493(5)
_cell_length_b                   16.2996(5)
_cell_length_c                   14.6770(5)
_cell_measurement_reflns_used    9569
_cell_measurement_temperature    100.01
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.59
_cell_volume                     3174.02(18)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'XS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.01
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0571
_diffrn_reflns_av_unetI/netI     0.0787
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            35982
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.519
_diffrn_reflns_theta_min         2.499
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.877
_exptl_absorpt_correction_T_max  0.0949
_exptl_absorpt_correction_T_min  0.0572
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1443 before and 0.0844 after correction.
The Ratio of minimum to maximum transmission is 0.6027.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_description       block
_exptl_crystal_F_000             1308
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.482
_refine_diff_density_min         -1.434
_refine_diff_density_rms         0.091
_refine_ls_abs_structure_details
;
 Flack x determined using 5182 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.012(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     706
_refine_ls_number_reflns         14102
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0533
_refine_ls_R_factor_gt           0.0447
_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^)+(0.0389P)^2^+2.2198P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1052
_refine_ls_wR_factor_ref         0.1111
_reflns_Friedel_coverage         0.864
_reflns_Friedel_fraction_full    0.942
_reflns_Friedel_fraction_max     0.927
_reflns_number_gt                12511
_reflns_number_total             14102
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00052h2.cif
_cod_data_source_block           20230110_prph3_0m
_cod_depositor_comments
'Adding full bibliography for 7715412--7715414.cif.'
_cod_database_code               7715413
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.957
_shelx_estimated_absorpt_t_min   0.957
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Rigid bond restraints
 C32, O5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C26) \\sim Ueq, Uanis(C58) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C41)
\\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C59) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.01
Uanis(C29) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
4.a Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B), C28(H28A,H28B), C30(H30A,H30B), C32(H32A,H32B), C58(H58A,
 H58B), C60(H60A,H60B), C68(H68A,H68B), C9(H9A,H9B), C37(H37A,H37B), C19(H19A,
 H19B), C41(H41A,H41B), C29(H29A,H29B), C15(H15A,H15B), C61(H61A,H61B),
 C31(H31A,H31B), C63(H63A,H63B)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C6(H6), C8(H8), C10(H10), C12(H12), C16(H16), C18(H18), C20(H20),
 C22(H22), C24(H24), C36(H36), C40(H40), C44(H44), C46(H46), C50(H50), C52(H52),
  C54(H54), C56(H56), C62(H62), C64(H64), C66(H66), C70(H70), C35(H35),
 C39(H39), C5(H5), C21(H21), C43(H43), C11(H11), C23(H23), C47(H47), C3(H3),
 C49(H49), C51(H51), C13(H13), C53(H53), C27(H27), C55(H55), C7(H7), C57(H57),
 C59(H59), C65(H65), C33(H33), C67(H67), C17(H17), C69(H69)
4.c Fitted hexagon refined as free rotating group:
 C8(C10,C12,C14,C16,C18), C47(C3,C49,C25,C51,C13)
;
_shelx_res_checksum              12464
_olex2_submission_special_instructions 'No special instructions were received'