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_7223514
_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
'2(C84 H70 Dy2 N12 Ni2 O31), 3(C3 H7 N O), C4 H10 O'
_chemical_formula_sum            'C181 H171 Dy4 N27 Ni4 O66'
_chemical_formula_weight         4665.28
_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   mixed
_audit_creation_date             2014-12-08
_audit_creation_method
;
Olex2 1.2
(compiled 2014.11.28 svn.r3106 for OlexSys, GUI svn.r4959)
;
_audit_update_record
;
2015-11-15 deposited with the CCDC.
2015-12-17 downloaded from the CCDC.
;
_cell_angle_alpha                98.527(3)
_cell_angle_beta                 98.268(3)
_cell_angle_gamma                111.403(4)
_cell_formula_units_Z            1
_cell_length_a                   14.1586(6)
_cell_length_b                   17.2590(7)
_cell_length_c                   22.3936(8)
_cell_measurement_reflns_used    10941
_cell_measurement_temperature    173
_cell_measurement_theta_max      29.1600
_cell_measurement_theta_min      3.7600
_cell_volume                     4920.7(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      173
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1033
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.809
_diffrn_measurement_details
;
  1 omega  -82.00   11.00   1.0000   15.1400
omega____ theta____ kappa____ phi______ frames
    -      -16.1295  -77.0000  -60.0000 93

  2 omega  -33.00   51.00   1.0000   15.1400
omega____ theta____ kappa____ phi______ frames
    -      -16.1295   57.0000 -180.0000 84

  3 omega  -43.00   48.00   1.0000   15.1400
omega____ theta____ kappa____ phi______ frames
    -      -16.1295   77.0000   60.0000 91

  4 omega   -3.00   47.00   1.0000   15.1400
omega____ theta____ kappa____ phi______ frames
    -       16.7545  -99.0000 -150.0000 50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0028415000
_diffrn_orient_matrix_UB_12      -0.0061424000
_diffrn_orient_matrix_UB_13      0.0307271000
_diffrn_orient_matrix_UB_21      0.0092465000
_diffrn_orient_matrix_UB_22      -0.0373109000
_diffrn_orient_matrix_UB_23      -0.0090075000
_diffrn_orient_matrix_UB_31      0.0542397000
_diffrn_orient_matrix_UB_32      0.0248144000
_diffrn_orient_matrix_UB_33      0.0070862000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0315
_diffrn_reflns_av_unetI/netI     0.0630
_diffrn_reflns_laue_measured_fraction_full 0.984
_diffrn_reflns_laue_measured_fraction_max 0.809
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            33792
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.809
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.414
_diffrn_reflns_theta_min         3.357
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.966
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38858
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
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    1.574
_exptl_crystal_description       block
_exptl_crystal_F_000             2350
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.322
_refine_diff_density_min         -0.928
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1284
_refine_ls_number_reflns         21989
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0618
_refine_ls_R_factor_gt           0.0425
_refine_ls_shift/su_max          0.030
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0415P)^2^+2.4718P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0968
_refine_ls_wR_factor_ref         0.1096
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17058
_reflns_number_total             21989
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce02109j3.cif
_cod_data_source_block           21_CCDC_1406237
_cod_depositor_comments
'Adding full bibliography for 7223506--7223525.cif.'
_cod_database_code               7223514
_shelxl_version_number           2014-1
_chemical_oxdiff_formula         C80H60N8O20Ni2Dy2
_reflns_odcompleteness_completeness 98.37
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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
2. Restrained distances
 C98-C97
 1.53 with sigma of 0.02
 C96-C95
 1.53 with sigma of 0.02
 C96-O24
 1.43 with sigma of 0.02
 O24-C97
 1.43 with sigma of 0.02
 C91-N14
 1.46 with sigma of 0.02
 N6-C94
 1.46 with sigma of 0.02
 N6-C64
 1.46 with sigma of 0.02
 N8-C93
 1.46 with sigma of 0.02
 N8-C70
 1.46 with sigma of 0.02
3. Restrained planarity
 O34, C90, N14, C91, C92
 with sigma of 0.1
 O26, C68, N8, C70, C69
 with sigma of 0.1
 O26, C68, N8, C69, C93
 with sigma of 0.1
 O17, C62, N6, C63, C64
 with sigma of 0.1
 C62, O17, N6, C94, C63
 with sigma of 0.1
4. Others
 Fixed Sof: C94(0.5) H94A(0.5) H94B(0.5) H94C(0.5) C70(0.5) H70A(0.5)
 H70B(0.5) H70C(0.5) C92(0.5) H92A(0.5) H92B(0.5) H92C(0.5) N14(0.5) C90(0.5)
 H90(0.5) O34(0.5) C91(0.5) H91A(0.5) H91B(0.5) H91C(0.5) O24(0.5) C97(0.5)
 H97A(0.5) H97B(0.5) C95(0.5) H95A(0.5) H95B(0.5) H95C(0.5) C96(0.5) H96A(0.5)
 H96B(0.5) C98(0.5) H24(0.5) H98A(0.5) H98B(0.5) C64(0.5) H64A(0.5) H64B(0.5)
 H64C(0.5) C93(0.5) H93A(0.5) H93B(0.5) H93C(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C97(H97A,H97B), C96(H96A,H96B)
5.b Aromatic/amide H refined with riding coordinates:
 C44(H44), C53(H53), C35(H35), C46(H46), C10(H10), C17(H17), C8(H8), C12(H12),
 C26(H26), C3(H3), C28(H28), C13(H13), C75(H75), C61(H61), C33(H33), C32(H32),
 C87(H87), C48(H48), C5(H5), C57(H57), C14(H14), C4(H4), C15(H15), C49(H49),
 C50(H50), C21(H21), C31(H31), C79(H79), C39(H39), C51(H51), C59(H59), C77(H77),
  C41(H41), C30(H30), C22(H22), C86(H86), C62(H62), C65(H65), C82(H82),
 C23(H23), C40(H40), C84(H84), C68(H68), C90(H90)
5.c Idealised Me refined as rotating group:
 C37(H37A,H37B,H37C), C1(H1A,H1B,H1C), C19(H19A,H19B,H19C), C88(H88A,H88B,
 H88C), C89(H89A,H89B,H89C), C69(H69A,H69B,H69C), C63(H63A,H63B,H63C), C94(H94A,
 H94B,H94C), C66(H66A,H66B,H66C), C70(H70A,H70B,H70C), C92(H92A,H92B,H92C),
 C67(H67A,H67B,H67C), C91(H91A,H91B,H91C), C95(H95A,H95B,H95C), C98(H24,H98A,
 H98B), C64(H64A,H64B,H64C), C93(H93A,H93B,H93C)
;
_olex2_submission_special_instructions 'No special instructions were received'