Synthesis, structure, and magnetism of non-planar heptanuclear lanthanide(III) complexes.
Goura, Joydeb; Walsh, James P. S.; Tuna, Floriana; Chandrasekhar, Vadapalli; Dalton transactions (Cambridge, England : 2003) 44 (2015) 1142–1149; doi:10.1039/c4dt01603c

data_7033022
_publ_section_title
;
 Synthesis, structure, and magnetism of non-planar heptanuclear
 lanthanide(III) complexes.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1142
_journal_page_last               1149
_journal_paper_doi               10.1039/c4dt01603c
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C78 H72 N22 O32 Tb7, 3(N O3)'
_chemical_formula_sum            'C78 H72 N25 O41 Tb7'
_chemical_formula_weight         3128.04
_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             2014-10-30
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_cell_angle_alpha                104.849(5)
_cell_angle_beta                 94.612(5)
_cell_angle_gamma                95.967(5)
_cell_formula_units_Z            2
_cell_length_a                   15.215(5)
_cell_length_b                   16.425(5)
_cell_length_c                   24.769(5)
_cell_measurement_reflns_used    9820
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.349
_cell_measurement_theta_min      2.279
_cell_volume                     5914(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.955
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0506
_diffrn_reflns_av_unetI/netI     0.1001
_diffrn_reflns_Laue_measured_fraction_full 0.955
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            46813
_diffrn_reflns_point_group_measured_fraction_full 0.955
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_min         4.103
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.213
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5623
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.1022 before and 0.0546 after correction. The Ratio of minimum to maximum transmission is 0.7541. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.757
_exptl_crystal_description       block
_exptl_crystal_F_000             2996
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         5.618
_refine_diff_density_min         -1.575
_refine_diff_density_rms         0.256
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1336
_refine_ls_number_reflns         20448
_refine_ls_number_restraints     2298
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0934
_refine_ls_R_factor_gt           0.0703
_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^)+(0.0907P)^2^+54.2183P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1771
_refine_ls_wR_factor_ref         0.1882
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14990
_reflns_number_total             20448
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt01603c2.cif
_cod_data_source_block           Tb7
_cod_depositor_comments
'Adding full bibliography for 7033021--7033025.cif.'
_cod_database_code               7033022
_shelxl_version_number           2014/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O1A-N74 = N74-O65
 1.205 with sigma of 0.02
 O1A-N74 = N74-O66
 1.205 with sigma of 0.02
 O66-N74 = N74-O65
 1.205 with sigma of 0.02
 O1A-O65
 2.087 with sigma of 0.04
 O1A-O66
 2.087 with sigma of 0.04
 O66-O65
 2.087 with sigma of 0.04
 O1A-N74 \\sim N74-O65
 with sigma of 0.02
 O1C-N1A \\sim N1A-O1B
 with sigma of 0.02
 O1B-N1A \\sim N1A-O1D
 with sigma of 0.02
 O1D-N1A \\sim N1A-O1C
 with sigma of 0.02
 O1C-O1B \\sim O1B-O1D
 with sigma of 0.02
3. Restrained planarity
 O65, N74, O1A, O66
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(N9) = Uanis(C35) = Uanis(N8)
Uanis(O1A) = Uanis(N74) = Uanis(O65)
Uanis(O66) = Uanis(N74) = Uanis(O1A) = Uanis(O65)
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Aromatic/amide H refined with riding coordinates:
 N2(H2), N5(H5), N8(H8), N11(H11), N14(H14), N17(H17), C3(H3), C4(H4), C5(H5A),
  C8(H8A), C10(H10), C11(H11A), C12(H12), C13(H13), C16(H16), C17(H17A),
 C18(H18), C21(H21), C23(H23), C24(H24), C25(H25), C26(H26), C29(H29), C30(H30),
  C31(H31), C34(H34), C36(H36), C37(H37), C38(H38), C39(H39), C42(H42),
 C43(H43), C44(H44), C47(H47), C49(H49), C50(H50), C51(H51), C52(H52), C55(H55),
  C56(H56), C57(H57), C60(H60), C62(H62), C63(H63), C64(H64), C65(H65),
 C68(H68), C69(H69), C70(H70), C72(H72), C74(H74), C75(H75), C76(H76), C77(H77)
6.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C14(H14A,H14B,H14C), C27(H27A,H27B,H27C), C40(H40A,H40B,
 H40C), C53(H53A,H53B,H53C), C66(H66A,H66B,H66C)
;
_olex2_submission_special_instructions 'No special instructions were received'