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_7223522
_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
'C110 H102 Dy2 N4 Ni2 O20, 2(C4 H8 O) 2(C2 H6 O)'
_chemical_formula_sum            'C122 H130 Dy2 N4 Ni2 O24'
_chemical_formula_weight         2478.64
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2015-01-10
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            9
_cell_length_a                   38.159(3)
_cell_length_b                   38.159(3)
_cell_length_c                   18.7654(13)
_cell_measurement_temperature    100
_cell_volume                     23664(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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.992
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0483
_diffrn_reflns_av_unetI/netI     0.0370
_diffrn_reflns_laue_measured_fraction_full 0.990
_diffrn_reflns_laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       49
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -49
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            56666
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.483
_diffrn_reflns_theta_min         2.496
_exptl_absorpt_coefficient_mu    1.832
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.723
_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. Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm'
_exptl_crystal_colour            'dark orange'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.507
_exptl_crystal_description       prism
_exptl_crystal_F_000             10962
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.455
_refine_diff_density_min         -0.895
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     638
_refine_ls_number_reflns         11972
_refine_ls_number_restraints     73
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.0553
_refine_ls_R_factor_gt           0.0408
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0768P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1095
_refine_ls_wR_factor_ref         0.1157
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9239
_reflns_number_total             11972
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce02109j2.cif
_cod_data_source_block           9_CCDC_1406225
_cod_depositor_comments
'Adding full bibliography for 7223506--7223525.cif.'
_cod_original_cell_volume        23664(4)
_cod_database_code               7223522
_shelxl_version_number           2014-1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O23-H23
 0.85 with sigma of 0.01
 C728-H23
 1.886514 with sigma of 0.02
 Ni13-H23
 2.587601 with sigma of 0.02
3. Rigid bond restraints
 O3, C8, C10, C5, C6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
H126 \\sim O3 \\sim C8 \\sim C10 \\sim C5 \\sim C6: within 1.7A with sigma of
0.04 and sigma for terminal atoms of 0.08
Uanis(C755) = Uanis(C2) = Uanis(C551)
Uanis(C4) = Uanis(C53) = Uanis(C9)
Uanis(C212) = Uanis(C307) = Uanis(C58)
5. Rigid body (RIGU) restrains
 O3, C8, C10, C5, C6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C5(H5A,H5B), C6(H6A,H6B)
6.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C212(H21A,H21B), C551(H55A,H55B), C728(H72A,H72B)
6.c Aromatic/amide H refined with riding coordinates:
 C80(H80), C239(H239), C16(H16), C29(H29), C53(H53), C110(H110), C126(H126),
 C2(H2), C18(H18), C46(H46), C59(H59), C168(H168), C1(H1), C307(H307),
 C321(H321), C360(H360), C379(H379), C411(H411), C422(H422), C469(H469),
 C504(H504), C635(H635), C716(H716), C757(H757)
6.d X=CH2 refined with riding coordinates:
 C58(H58A,H58B), C755(H75A,H75B)
6.e Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C345(H34A,H34B,H34C), C674(H67A,H67B,H67C), C7(H7A,H7B,
 H7C)
;
_shelx_res_checksum              40079
_olex2_submission_special_instructions 'No special instructions were received'