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_7033023
_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 Dy7 N22 O32, 3(N O3)'
_chemical_formula_sum            'C78 H72 Dy7 N25 O41'
_chemical_formula_weight         3153.10
_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                104.542(5)
_cell_angle_beta                 97.034(5)
_cell_angle_gamma                92.794(5)
_cell_formula_units_Z            2
_cell_length_a                   14.813(5)
_cell_length_b                   16.161(5)
_cell_length_c                   24.410(5)
_cell_measurement_reflns_used    9909
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.268
_cell_measurement_theta_min      2.374
_cell_volume                     5595(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 0.967
_diffrn_measured_fraction_theta_max 0.991
_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  0.0803
_diffrn_reflns_av_unetI/netI     0.1453
_diffrn_reflns_Laue_measured_fraction_full 0.967
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            48248
_diffrn_reflns_point_group_measured_fraction_full 0.967
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_min         4.107
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.703
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5355
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0882 before and 0.0512 after correction.
The Ratio of minimum to maximum transmission is 0.7181.
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    1.872
_exptl_crystal_description       block
_exptl_crystal_F_000             3010
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         4.539
_refine_diff_density_min         -2.829
_refine_diff_density_rms         0.225
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1330
_refine_ls_number_reflns         19595
_refine_ls_number_restraints     2292
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0996
_refine_ls_R_factor_gt           0.0616
_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^)+(0.0721P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1430
_refine_ls_wR_factor_ref         0.1535
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12955
_reflns_number_total             19595
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt01603c2.cif
_cod_data_source_block           Dy7
_cod_depositor_comments
'Adding full bibliography for 7033021--7033025.cif.'
_cod_database_code               7033023
_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-O1F
 with sigma of 0.02
 O1F-N1A \\sim N1A-O1D
 with sigma of 0.02
 O1D-O1E \\sim O1E-O1F
 with sigma of 0.02
 O1B-O1A \\sim O1A-O1C
 with sigma of 0.02
 O1E-O1D \\sim O1D-O1F
 with sigma of 0.02
3. Restrained planarity
 O1A, O1B, N1B, O1C
 with sigma of 0.1
 O1E, N1A, O1F, O1D
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
O1C \\sim N1B \\sim O1A: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
O1A \\sim N1B \\sim O1B: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
O1B \\sim N1B \\sim O1C: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
O1C \\sim O1A \\sim O1B: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
Uanis(O1E) = Uanis(N1A) = Uanis(O1F) = Uanis(O1D)
Uanis(O1B) = Uanis(N1B) = Uanis(O1C) = Uanis(O1A)
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),
  C6(H6), C9(H9), C11(H11A), C12(H12), C13(H13), C14(H14A), C17(H17A), C18(H18),
  C19(H19), C22(H22), C24(H24), C25(H25), C28(H28), C29(H29), C30(H30),
 C33(H33), C35(H35), C36(H36), C37(H37), C38(H38), C41(H41), C42(H42), C43(H43),
  C46(H46), C48(H48), C49(H49), C50(H50), C51(H51), C54(H54), C55(H55),
 C56(H56), C59(H59), C61(H61), C62(H62), C63(H63), C66(H66), C67(H67), C68(H68),
  C71(H71), C73(H73), C74(H74), C75(H75), C76(H76), C77(H77), C78(H78)
6.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C15(H15A,H15B,H15C), C26(H26A,H26B,H26C), C39(H39A,H39B,
 H39C), C52(H52A,H52B,H52C), C64(H64A,H64B,H64C)
;
_olex2_submission_special_instructions 'No special instructions were received'