Heterometallic Ln-Cu complexes derived from a phenyl pyrimidyl substituted nitronyl nitroxide biradical.
Wang, Kang; Sun, Juan; Xi, Lu; Lu, Jiao; Jing, Pei; Li, Licun; Dalton transactions (Cambridge, England : 2003) 48 (2019) 14383–14389; doi:10.1039/c9dt03081f

data_7700972
_publ_section_title
;
 Heterometallic Ln-Cu complexes derived from a phenyl pyrimidyl
 substituted nitronyl nitroxide biradical.
;
_journal_issue                   38
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14383
_journal_page_last               14389
_journal_paper_doi               10.1039/c9dt03081f
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C49 H35 Cu F30 N6 O14 Tb'
_chemical_formula_sum            'C49 H35 Cu F30 N6 O14 Tb'
_chemical_formula_weight         1724.29
_chemical_name_systematic        Tb-Cu
_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     direct
_audit_creation_date             2019-05-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-07-27 deposited with the CCDC.    2019-08-29 downloaded from the CCDC.
;
_cell_angle_alpha                66.608(14)
_cell_angle_beta                 74.109(12)
_cell_angle_gamma                69.007(11)
_cell_formula_units_Z            2
_cell_length_a                   12.7313(14)
_cell_length_b                   16.474(2)
_cell_length_c                   18.826(3)
_cell_measurement_reflns_used    5161
_cell_measurement_temperature    113
_cell_measurement_theta_max      24.6650
_cell_measurement_theta_min      3.4660
_cell_volume                     3343.3(9)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      113
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2116
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.837
_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    -51.00  63.00   1.00   16.50    --   18.63 -19.00 -60.00  114
  2  \w    -19.00   8.00   1.00   16.50    --   18.63 -99.00  60.00   27
  3  \w     20.00  60.00   1.00   16.50    --   18.63 -99.00  60.00   40
  4  \w    -52.00   9.00   1.00   16.50    --  -19.72 -77.00 150.00   61
  5  \w    -90.00  10.00   1.00   16.50    --  -19.72 -77.00 -90.00  100
  6  \w    -31.00  45.00   1.00   16.50    --  -19.72  77.00  90.00   76
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0179643000
_diffrn_orient_matrix_UB_12      -0.0000063000
_diffrn_orient_matrix_UB_13      -0.0324903000
_diffrn_orient_matrix_UB_21      -0.0210011000
_diffrn_orient_matrix_UB_22      -0.0382291000
_diffrn_orient_matrix_UB_23      0.0244624000
_diffrn_orient_matrix_UB_31      -0.0536958000
_diffrn_orient_matrix_UB_32      0.0305039000
_diffrn_orient_matrix_UB_33      0.0084765000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0452
_diffrn_reflns_av_unetI/netI     0.0985
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.837
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            28437
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.837
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.302
_diffrn_reflns_theta_min         2.874
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.513
_exptl_absorpt_correction_T_max  0.762
_exptl_absorpt_correction_T_min  0.724
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.713
_exptl_crystal_description       prism
_exptl_crystal_F_000             1694
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.864
_refine_diff_density_min         -0.929
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     921
_refine_ls_number_reflns         15312
_refine_ls_number_restraints     844
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.1282
_refine_ls_R_factor_gt           0.0759
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1032P)^2^+6.9155P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1858
_refine_ls_wR_factor_ref         0.2259
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9191
_reflns_number_total             15312
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03081f2.cif
_cod_data_source_block           tb-cu
_cod_depositor_comments
'Adding full bibliography for 7700970--7700972.cif.'
_cod_original_cell_volume        3343.2(9)
_cod_database_code               7700972
_shelx_shelxl_version_number     2014/7
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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. Restrained distances
 H14A-H17A
 2.35 with sigma of 0.01
 C13-C17
 1.5 with sigma of 0.02
3. Rigid bond restraints
 C12, C15
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.005
 C12, C14
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
C31 \\sim C4 \\sim C3 \\sim C2 \\sim C5 \\sim C43 \\sim C8 \\sim C10 \\sim C1
\\sim C46 \\sim C6 \\sim C9 \\sim C38 \\sim C18 \\sim C7 \\sim C28 \\sim C30
\\sim C19 \\sim C11 \\sim C37 \\sim C32 \\sim C47 \\sim C36 \\sim C26 \\sim C45
\\sim C35 \\sim C12 \\sim C39 \\sim C27 \\sim C48 \\sim C22 \\sim C33 \\sim C40
\\sim C29 \\sim C24 \\sim C41 \\sim C23 \\sim C20 \\sim C25 \\sim C21 \\sim C13
\\sim C42 \\sim C17 \\sim C49 \\sim C44 \\sim C16 \\sim C14 \\sim C15 \\sim
C34: within 3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02
C12 \\sim C15 \\sim C14: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C17) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C14) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C16) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(F11) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C15) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(F12) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
5.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C2(H2), C8(H8), C10(H10), C1(H1), C6(H6), C37(H37), C32(H32),
 C47(H47), C27(H27), C42(H42)
5.b Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C23(H23A,H23B,H23C), C21(H21A,H21B,
 H21C), C17(H17A,H17B,H17C), C16(H16A,H16B,H16C), C14(H14A,H14B,H14C), C15(H15A,
 H15B,H15C)
;
_shelx_res_checksum              16362
_shelx_fab_checksum              21458
_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 1.310
_oxdiff_exptl_absorpt_empirical_full_min 0.766