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_7700971
_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 Dy F30 N6 O14'
_chemical_formula_sum            'C49 H35 Cu Dy F30 N6 O14'
_chemical_formula_weight         1727.87
_chemical_name_systematic        Dy-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                65.678(9)
_cell_angle_beta                 74.451(7)
_cell_angle_gamma                68.870(6)
_cell_formula_units_Z            2
_cell_length_a                   12.7276(9)
_cell_length_b                   16.6594(11)
_cell_length_c                   18.6223(19)
_cell_measurement_reflns_used    4782
_cell_measurement_temperature    113
_cell_measurement_theta_max      22.4850
_cell_measurement_theta_min      3.3060
_cell_volume                     3322.8(5)
_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_temperature      113
_diffrn_detector_area_resol_mean 16.2116
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0534
_diffrn_reflns_av_unetI/netI     0.1103
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            22059
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        25.010
_diffrn_reflns_theta_max         25.010
_diffrn_reflns_theta_min         2.901
_exptl_absorpt_coefficient_mu    1.582
_exptl_absorpt_correction_T_max  0.729
_exptl_absorpt_correction_T_min  0.702
_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    1.727
_exptl_crystal_description       prism
_exptl_crystal_F_000             1696
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.20
_refine_diff_density_max         4.537
_refine_diff_density_min         -1.140
_refine_diff_density_rms         0.156
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     921
_refine_ls_number_reflns         11431
_refine_ls_number_restraints     823
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.1623
_refine_ls_R_factor_gt           0.1032
_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^)+(0.1484P)^2^+17.7032P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2457
_refine_ls_wR_factor_ref         0.3063
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6527
_reflns_number_total             11431
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03081f2.cif
_cod_data_source_block           dy-cu
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7700970--7700972.cif.
;
_cod_database_code               7700971
_shelx_shelxl_version_number     2014/7
_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
 H15A-H16C
 2.35 with sigma of 0.01
3. Rigid bond restraints
 F22, C44
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.005
 F23, C44
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.005
 C15, C12
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.005
 F28, C49
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.005
 C49, F30
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F12, C34
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
C2 \\sim C44 \\sim C3 \\sim C4 \\sim C6 \\sim C28 \\sim C5 \\sim C9 \\sim C10
\\sim C46 \\sim C1 \\sim C38 \\sim C7 \\sim C8 \\sim C36 \\sim C45 \\sim C43
\\sim C18 \\sim C19 \\sim C12 \\sim C35 \\sim C11 \\sim C37 \\sim C39 \\sim C48
\\sim C42 \\sim C26 \\sim C29 \\sim C47 \\sim C49 \\sim C40 \\sim C23 \\sim C27
\\sim C41 \\sim C24 \\sim C15 \\sim C22 \\sim C25 \\sim C20 \\sim C14 \\sim C21
\\sim C17 \\sim C13 \\sim C16 \\sim C34 \\sim C31 \\sim C30 \\sim C32 \\sim
C33: within 3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02
C17 \\sim C13 \\sim C16: 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(F11) \\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:
 C2(H2), C4(H4), C6(H6), C10(H10), C1(H1), C8(H8), C37(H37), C42(H42),
 C47(H47), C27(H27), C32(H32)
5.b Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C15(H15A,H15B,H15C), C22(H22A,H22B,
 H22C), C14(H14A,H14B,H14C), C21(H21A,H21B,H21C), C17(H17A,H17B,H17C), C16(H16A,
 H16B,H16C)
;
_shelx_res_checksum              47022
_shelx_fab_checksum              6251
_olex2_submission_special_instructions 'No special instructions were received'