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_7223510
_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         'C62 H58 Dy2 N4 Ni2 O18'
_chemical_formula_sum            'C62 H58 Dy2 N4 Ni2 O18'
_chemical_formula_weight         1589.54
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2015-11-14
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2015-11-15 deposited with the CCDC.
2015-12-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.977(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.4776(4)
_cell_length_b                   21.3408(8)
_cell_length_c                   14.3681(5)
_cell_measurement_reflns_used    2917
_cell_measurement_temperature    173
_cell_measurement_theta_max      70.2570
_cell_measurement_theta_min      4.3630
_cell_volume                     3072.7(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      173
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1033
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_details
;
  1 omega -105.00   -8.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -      -36.2297  -77.0000  -30.0000 97

  2 omega  -36.00   69.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -       36.2297  -19.0000  150.0000 105

  3 omega   35.00   66.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -      106.0000  -30.0000   90.0000 31

  4 omega   38.00   65.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -      106.0000  -45.0000  -30.0000 27

  5 omega   35.00   68.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -      106.0000  -30.0000   30.0000 33

  6 omega   35.00   69.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -      106.0000  -30.0000  150.0000 34

  7 omega   48.00  123.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -      106.0000  -61.0000    0.0000 75

  8 omega   82.00  177.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -      106.0000   30.0000  -90.0000 95

  9 omega   58.00  115.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -      106.0000  -61.0000   90.0000 57

 10 omega   46.00  147.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -      106.0000  -15.0000  -90.0000 101
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.1236690000
_diffrn_orient_matrix_UB_12      0.0392048000
_diffrn_orient_matrix_UB_13      -0.0520880000
_diffrn_orient_matrix_UB_21      -0.0135810000
_diffrn_orient_matrix_UB_22      0.0210525000
_diffrn_orient_matrix_UB_23      0.0992092000
_diffrn_orient_matrix_UB_31      0.0901923000
_diffrn_orient_matrix_UB_32      0.0569080000
_diffrn_orient_matrix_UB_33      -0.0008444000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0927
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.441
_diffrn_reflns_theta_min         4.875
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    14.105
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.40372
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.718
_exptl_crystal_description       block
_exptl_crystal_F_000             1580
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         3.244
_refine_diff_density_min         -1.358
_refine_diff_density_rms         0.222
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.990
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     386
_refine_ls_number_reflns         5641
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.991
_refine_ls_R_factor_all          0.0899
_refine_ls_R_factor_gt           0.0666
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1092P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1672
_refine_ls_wR_factor_ref         0.1837
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4122
_reflns_number_total             5641
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce02109j3.cif
_cod_data_source_block           17_CCDC_1406233
_cod_depositor_comments
'Adding full bibliography for 7223506--7223525.cif.'
_cod_database_code               7223510
_shelxl_version_number           2014-1
_chemical_oxdiff_formula         'Ni2 Dy2 C80 H80 O20 N10'
_reflns_odcompleteness_completeness 98.68
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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, All O(H) groups
2. Restrained distances
 O9-H9
 0.87 with sigma of 0.01
 C31-H9
 1.905692 with sigma of 0.02
 Dy1-H9
 3.001359 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C31) = Uanis(O9) = Uanis(C15) = Uanis(O4)
4.a Aromatic/amide H refined with riding coordinates:
 C26(H26), C11(H11), C24(H24), C18(H18), C12(H12), C17(H17), C13(H13), C3(H3),
 C25(H25), C22(H22), C4(H4), C27(H27), C19(H19), C5(H5), C10(H10), C8(H8)
4.b Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C31(H31A,H31B,H31C), C1(H1A,H1B,H1C), C30(H30A,H30B,H30C)
;
_olex2_submission_special_instructions 'No special instructions were received'