Magnetic anisotropy investigation on light lanthanide complexes.
Xu, Mei-Xing; Meng, Yin-Shan; Xiong, Jin; Wang, Bing-Wu; Jiang, Shang-Da; Gao, Song; Dalton transactions (Cambridge, England : 2003) 47 (2018) 1966–1971; doi:10.1039/c7dt04351a

data_7045185
_publ_section_title
;
 Magnetic anisotropy investigation on light lanthanide complexes.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1966
_journal_page_last               1971
_journal_paper_doi               10.1039/c7dt04351a
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C34 H38 F9 N2 O6 Pr'
_chemical_formula_sum            'C34 H38 F9 N2 O6 Pr'
_chemical_formula_weight         882.57
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-11-01
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5335)
;
_audit_update_record
;
2017-11-18 deposited with the CCDC.
2017-12-29 downloaded from the CCDC.
;
_cell_angle_alpha                99.871(2)
_cell_angle_beta                 103.967(3)
_cell_angle_gamma                101.416(3)
_cell_formula_units_Z            2
_cell_length_a                   9.5517(3)
_cell_length_b                   12.2277(4)
_cell_length_c                   17.9577(5)
_cell_measurement_reflns_used    9168
_cell_measurement_temperature    180.00(10)
_cell_measurement_theta_max      27.4950
_cell_measurement_theta_min      3.2650
_cell_volume                     1941.40(11)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      180.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3914
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega    7.00   72.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       10.5454 -131.0000  -17.7693 65

  2 omega  -25.00    7.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       10.5454  -38.0000 -120.0000 32

  3 omega  -19.00   89.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       10.5454   77.0000  -60.0000 108

  4 omega  -16.00   77.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       10.5454   38.0000 -150.0000 93

  5 omega  -16.00   86.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       10.5454   38.0000   90.0000 102

  6 omega  -63.00   37.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       10.5454  -38.0000   30.0000 100

  7 omega  -19.00   31.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       10.5454  -99.0000  150.0000 50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0554508000
_diffrn_orient_matrix_UB_12      0.0293237000
_diffrn_orient_matrix_UB_13      0.0047923000
_diffrn_orient_matrix_UB_21      -0.0538957000
_diffrn_orient_matrix_UB_22      -0.0532245000
_diffrn_orient_matrix_UB_23      -0.0101969000
_diffrn_orient_matrix_UB_31      0.0163499000
_diffrn_orient_matrix_UB_32      -0.0024093000
_diffrn_orient_matrix_UB_33      0.0402816000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71000
_diffrn_reflns_av_R_equivalents  0.0434
_diffrn_reflns_av_unetI/netI     0.0487
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            25888
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         3.19
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.341
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77945
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.510
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             888
_refine_diff_density_max         1.140
_refine_diff_density_min         -0.455
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     478
_refine_ls_number_reflns         7640
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0454
_refine_ls_R_factor_gt           0.0336
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0269P)^2^+1.6351P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0690
_refine_ls_wR_factor_ref         0.0751
_reflns_number_gt                6550
_reflns_number_total             7640
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7dt04351a3.cif
_cod_data_source_block           161113_1_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7045184--7045186.cif.'
_cod_original_cell_volume        1941.39(10)
_cod_database_code               7045185
_chemical_oxdiff_formula         'C20 H6 F12 Pr1 N2'
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C0AA(H0AA), C16(H16), C21(H21), C30(H30), C31(H31), C35(H35), C39(H39),
 C47(H47), C49(H49), C55(H55), C58(H58)
2.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C27(H27A,H27B,H27C),
 C43(H43A,H43B,H43C), C51(H51A,H51B,H51C), C61(H61A,H61B,H61C), C70(H70A,H70B,
 H70C), C78(H78A,H78B,H78C)
;
_olex2_submission_special_instructions 'No special instructions were received'