Isoskeletal Schiff base polynuclear coordination clusters: synthetic and theoretical aspects
Griffiths, Kieran; Dokorou, Vassiliki N.; Spencer, John; Abdul-Sada, Alaa; Vargas, Alfredo; Kostakis, George E.; CrystEngComm 18 (2016) 704–; doi:10.1039/C5CE02109J

data_7223513
_publ_section_title
;
 Isoskeletal Schiff base polynuclear coordination clusters: synthetic and
 theoretical aspects
;
_journal_issue                   5
_journal_name_full               CrystEngComm
_journal_page_first              704
_journal_paper_doi               10.1039/C5CE02109J
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         'C81 H69 Dy3 N24 O60'
_chemical_formula_sum            'C81 H69 Dy3 N24 O60'
_chemical_formula_weight         2826.10
_chemical_name_systematic
;
 ?
;
_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     iterative
_audit_creation_date             2015-01-09
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.06 svn.r3119 for OlexSys, GUI svn.r4979)
;
_audit_update_record
;
2015-11-15 deposited with the CCDC.
2015-12-17 downloaded from the CCDC.
;
_cell_angle_alpha                81.572(2)
_cell_angle_beta                 80.148(2)
_cell_angle_gamma                83.020(2)
_cell_formula_units_Z            2
_cell_length_a                   16.5657(12)
_cell_length_b                   17.6842(12)
_cell_length_c                   18.4698(13)
_cell_measurement_temperature    100
_cell_volume                     5247.5(6)
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.981
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0367
_diffrn_reflns_av_unetI/netI     0.0304
_diffrn_reflns_laue_measured_fraction_full 0.983
_diffrn_reflns_laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            76415
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.505
_diffrn_reflns_theta_min         2.340
_exptl_absorpt_coefficient_mu    2.233
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.803
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.789
_exptl_crystal_description       block
_exptl_crystal_F_000             2802
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.105
_refine_diff_density_min         -1.468
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1489
_refine_ls_number_reflns         23648
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0360
_refine_ls_R_factor_gt           0.0314
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0344P)^2^+11.8159P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0764
_refine_ls_wR_factor_ref         0.0797
_reflns_Friedel_coverage         0.000
_reflns_number_gt                21515
_reflns_number_total             23648
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce02109j3.cif
_cod_data_source_block           20_CCDC_1406236
_cod_depositor_comments
'Adding full bibliography for 7223506--7223525.cif.'
_cod_database_code               7223513
_shelxl_version_number           2014-1
_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. Uiso/Uaniso restraints and constraints
Uanis(C9) = Uanis(C6)
Uanis(O10) = Uanis(C4) = Uanis(N0AA) = Uanis(C9) = Uanis(C6)
Uanis(O5) = Uanis(O3) = Uanis(N3)
3.a Aromatic/amide H refined with riding coordinates:
 C124(H124), C12(H12), C34(H34), C40(H40), C22(H22), C29(H29), C35(H35),
 C42(H42), C45(H45), C50(H50), C53(H53), C56(H56), C63(H63), C85(H85), C89(H89),
  C91(H91), C94(H94), C96(H96), C105(H105), C108(H108), C110(H110), C112(H112),
 C113(H113), C116(H116), C123(H123), C126(H126), C131(H131), C142(H142),
 C143(H143), C145(H145), C156(H156), C158(H158), C4(H4)
3.b Idealised Me refined as rotating group:
 C114(H11A,H11B,H11C), C7(H7A,H7B,H7C), C18(H18A,H18B,H18C), C28(H28A,H28B,
 H28C), C2(H2A,H2B,H2C), C44(H44A,H44B,H44C), C79(H79A,H79B,H79C), C87(H87A,
 H87B,H87C), C138(H13A,H13B,H13C), C140(H14A,H14B,H14C), C6(H6A,H6B,H6C),
 C9(H9A,H9B,H9C)
;
_shelx_res_checksum              36968
_olex2_submission_special_instructions 'No special instructions were received'