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_7033024
_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 Ho7 N22 O32, 3(N O3)'
_chemical_formula_sum            'C78 H72 Ho7 N25 O41'
_chemical_formula_weight         3170.11
_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   mixed
_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                105.328(5)
_cell_angle_beta                 93.576(5)
_cell_angle_gamma                96.950(5)
_cell_formula_units_Z            2
_cell_length_a                   15.285(5)
_cell_length_b                   16.379(5)
_cell_length_c                   24.769(5)
_cell_measurement_reflns_used    8898
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.294
_cell_measurement_theta_min      2.283
_cell_volume                     5908(3)
_computing_cell_refinement       'SAINT v6.45A (Bruker, 2003)'
_computing_data_reduction        'SAINT v6.45A (Bruker, 2003)'
_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 0.979
_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     0.71069
_diffrn_reflns_av_R_equivalents  0.0341
_diffrn_reflns_av_unetI/netI     0.0813
_diffrn_reflns_Laue_measured_fraction_full 0.955
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            38639
_diffrn_reflns_point_group_measured_fraction_full 0.955
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_min         4.123
_exptl_absorpt_coefficient_mu    4.715
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.564007
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS v.2.10 (Bruker,2003) was used for absorption correction. R(int) was 0.0652 before and 0.0286 after correction. The Ratio of minimum to maximum transmission is 0.5640. 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    1.782
_exptl_crystal_description       block
_exptl_crystal_F_000             3024
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         3.247
_refine_diff_density_min         -1.907
_refine_diff_density_rms         0.234
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1342
_refine_ls_number_reflns         20438
_refine_ls_number_restraints     2290
_refine_ls_restrained_S_all      0.961
_refine_ls_R_factor_all          0.0700
_refine_ls_R_factor_gt           0.0524
_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^)+(0.0962P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1436
_refine_ls_wR_factor_ref         0.1548
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15059
_reflns_number_total             20438
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt01603c2.cif
_cod_data_source_block           Ho7
_cod_depositor_comments
'Adding full bibliography for 7033021--7033025.cif.'
_cod_database_code               7033024
_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
 O1D-N1A \\sim N1A-O1E
 with sigma of 0.02
 O1E-N1A \\sim N1A-O1C
 with sigma of 0.02
 O1C-N1A \\sim N1A-O1D
 with sigma of 0.02
 O1D-O1C \\sim O1C-O1E
 with sigma of 0.02
 O1A-N31 \\sim N31-O72
 with sigma of 0.02
 O1B-N31 \\sim N31-O1A
 with sigma of 0.02
 O1A-N31 \\sim N31-O72
 with sigma of 0.02
 O72-N31 \\sim N31-O1B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O1D) = Uanis(N1A) = Uanis(O1E) = Uanis(O1C)
Uanis(O1B) = Uanis(O1A)
4. 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
5.a Riding coordinates:
 N14(H14)
5.b Aromatic/amide H refined with riding coordinates:
 N2(H2), N8(H8), C17(H17), C21(H21), C13(H13), C16(H16), C39(H39), C4(H4),
 C51(H51), C49(H49), C42(H42), N5(H5), C37(H37), C50(H50), C44(H44), C62(H62),
 C52(H52), C8(H8A), C64(H64), N24(H24), C25(H25), C10(H10), C60(H60), N11(H11),
 C36(H36), C18(H18), C72(H72), C80(H80), C57(H57), C26(H26), C31(H31), C23(H23),
  C75(H75), C55(H55), C56(H56), C47(H47), C29(H29), C24(H24A), C3(H3), C65(H65),
  C34(H34), C77(H77), C5(H5A), C38(H38), C69(H69), C43(H43), C11(H11A),
 C74(H74), C12(H12), C76(H76), C30(H30), C68(H68), C63(H63)
5.c Idealised Me refined as rotating group:
 C66(H66A,H66B,H66C), C14(H14A,H14B,H14C), C40(H40A,H40B,H40C), C1(H1A,H1B,
 H1C), C53(H53A,H53B,H53C), C27(H27A,H27B,H27C)
;
_olex2_submission_special_instructions 'No special instructions were received'