Rhodamine-based field-induced single molecule magnets in Yb(iii) and Dy(iii) series
Huang, Wei; Xu, Jun; Wu, Dayu; Huang, Xingcai; Jiang, Jun; New J. Chem. 39 (2015) 8650–; doi:10.1039/C5NJ01724F

data_7055083
_publ_section_title
;
 Rhodamine-based field-induced single molecule magnets in Yb(iii) and
 Dy(iii) series
;
_journal_issue                   11
_journal_name_full               'New J. Chem.'
_journal_page_first              8650
_journal_paper_doi               10.1039/C5NJ01724F
_journal_volume                  39
_journal_year                    2015
_chemical_formula_moiety         'C72 H66 N10 O6 Yb, C H4 O, 0.5(H2 O), N O3'
_chemical_formula_sum            'C73 H71 N11 O10.5 Yb'
_chemical_formula_weight         1443.45
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-07-22
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-07-29 deposited with the CCDC.
2015-08-27 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 97.384(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.539(6)
_cell_length_b                   20.456(5)
_cell_length_c                   15.357(4)
_cell_measurement_reflns_used    6343
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      20.816
_cell_measurement_theta_min      2.237
_cell_volume                     7645(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0773
_diffrn_reflns_av_unetI/netI     0.0934
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            43835
_diffrn_reflns_theta_full        25.73
_diffrn_reflns_theta_max         25.73
_diffrn_reflns_theta_min         1.67
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.284
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.5619
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1423 before and 0.0656 after correction.
The Ratio of minimum to maximum transmission is 0.7539.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            dark-red
_exptl_crystal_density_diffrn    1.254
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2960
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.18
_platon_squeeze_details
;
;
_refine_diff_density_max         2.414
_refine_diff_density_min         -1.223
_refine_diff_density_rms         0.177
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     854
_refine_ls_number_reflns         14358
_refine_ls_number_restraints     1893
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.1256
_refine_ls_R_factor_gt           0.0802
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1447P)^2^+11.3627P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2181
_refine_ls_wR_factor_ref         0.2529
_reflns_number_gt                9228
_reflns_number_total             14358
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5nj01724f2.cif
_cod_data_source_block           complex1
_cod_depositor_comments
'Adding full bibliography for 7055083--7055087.cif.'
_cod_original_formula_sum        'C73 H71 N11 O10.50 Yb'
_cod_database_code               7055083
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All O(H) groups, All
  O(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C51-O7
 1.35 with sigma of 0.01
 N11-O11A = N11-O12A = N11-O13A = N11-O12 = N11-O11 = N11-O13
 1.34 with sigma of 0.01
 O11A-O12A = O12A-O13A = O13A-O11A
 2.22 with sigma of 0.02
3. Rigid bond restraints
 O13, O12, O11, O13A, O12A, O11A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N1, C35
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
O13 \\sim O12 \\sim O11 \\sim O13A \\sim O12A \\sim O11A: within 1.7A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17
\\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25
\\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33
\\sim C34 \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim C41 \\sim C42 \\sim C43
\\sim C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48 \\sim C49 \\sim C50 \\sim C88
\\sim C52 \\sim C53 \\sim C54 \\sim C55 \\sim C56 \\sim C57 \\sim C58 \\sim C59
\\sim C60 \\sim C61 \\sim C62 \\sim C63 \\sim C64 \\sim C65 \\sim C66 \\sim C67
\\sim C68 \\sim C69 \\sim C70 \\sim C71 \\sim C72 \\sim C35 \\sim C36 \\sim
C51: within 3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Sof(O13A)=Sof(O12A)=Sof(O11A)=1-FVAR(1)
 Sof(O13)=Sof(O12)=Sof(O11)=FVAR(1)
 Fixed Sof: O8(0.5) H8B(0.5) H8C(0.5)
6.a Riding coordinates:
 O7(H7B), O8(H8B,H8C)
6.b Secondary CH2 refined with riding coordinates:
 C33(H33A,H33B), C69(H69A,H69B), C71(H71A,H71B), C35(H35A,H35B)
6.c Me refined with riding coordinates:
 C22(H22A,H22B,H22C), C30(H30A,H30B,H30C), C34(H34A,H34B,H34C), C67(H67A,H67B,
 H67C), C68(H68A,H68B,H68C), C70(H70A,H70B,H70C), C72(H72A,H72B,H72C), C36(H36A,
 H36B,H36C)
6.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C7(H7), C8(H8), C10(H10), C13(H13), C14(H14),
 C15(H15), C16(H16), C20(H20), C24(H24), C27(H27), C31(H31), C39(H39), C40(H40),
  C41(H41), C43(H43), C44(H44), C46(H46), C49(H49), C50(H50), C88(H88),
 C52(H52), C56(H56), C59(H59), C62(H62), C65(H65), N1(H1), N2(H2), N3(H3A),
 N6(H6), N7(H7A), N8(H8A)
6.e Idealised Me refined as rotating group:
 C51(H51A,H51B,H51C)
;
_olex2_submission_special_instructions 'No special instructions were received'