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_7223520
_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 H118 Dy2 N10 Ni2 O18, 4(C3 H7 N O), 2(Cl O4)'
_chemical_formula_sum            'C122 H146 Cl2 Dy2 N14 Ni2 O30'
_chemical_formula_weight         2801.84
_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
_audit_creation_date             2014-07-29
_audit_creation_method
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_audit_update_record
;
2015-11-15 deposited with the CCDC.
2015-12-17 downloaded from the CCDC.
;
_cell_angle_alpha                100.291(8)
_cell_angle_beta                 106.198(7)
_cell_angle_gamma                105.143(5)
_cell_formula_units_Z            1
_cell_length_a                   12.5403(7)
_cell_length_b                   14.7915(10)
_cell_length_c                   18.880(2)
_cell_measurement_reflns_used    3730
_cell_measurement_temperature    173
_cell_measurement_theta_max      28.6500
_cell_measurement_theta_min      2.6630
_cell_volume                     3124.5(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_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      173.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1033
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.892
_diffrn_measurement_details
;
  1 omega  -44.00   52.00   1.0000   14.5000
omega____ theta____ kappa____ phi______ frames
    -      -18.0128   38.0000   90.0000 96

  2 omega    8.00   60.00   1.0000   14.5000
omega____ theta____ kappa____ phi______ frames
    -       18.3253  -99.0000  120.0000 52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0367260000
_diffrn_orient_matrix_UB_12      0.0488734000
_diffrn_orient_matrix_UB_13      0.0185765000
_diffrn_orient_matrix_UB_21      -0.0048156000
_diffrn_orient_matrix_UB_22      0.0092625000
_diffrn_orient_matrix_UB_23      -0.0361627000
_diffrn_orient_matrix_UB_31      -0.0501744000
_diffrn_orient_matrix_UB_32      0.0137674000
_diffrn_orient_matrix_UB_33      -0.0002509000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0478
_diffrn_reflns_av_unetI/netI     0.0683
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.892
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            9418
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.892
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.037
_diffrn_reflns_theta_min         2.478
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.602
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65587
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.489
_exptl_crystal_F_000             1438
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.24
_refine_diff_density_max         1.028
_refine_diff_density_min         -0.624
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     779
_refine_ls_number_reflns         7781
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0437
_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^)+(0.0527P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1070
_refine_ls_wR_factor_ref         0.1165
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6754
_reflns_number_total             7781
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce02109j2.cif
_cod_data_source_block           7_CCDC_1406223
_cod_depositor_comments
'Adding full bibliography for 7223506--7223525.cif.'
_cod_database_code               7223520
_shelxl_version_number           2014-1
_chemical_oxdiff_formula         Ni2Dy2C124H130N10O40
_reflns_odcompleteness_completeness 56.54
_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
 C9-C10 = C32-C33A
 1.29 with sigma of 0.02
 C32-C33
 1.29 with sigma of 0.02
 C33A-C32A
 1.29 with sigma of 0.02
 C33-C32
 1.29 with sigma of 0.02
 C8-C9 = C31A-C32A
 1.49 with sigma of 0.02
 C31-C32
 1.49 with sigma of 0.02
 C31A-C27
 1.49 with sigma of 0.02
 C31-C27
 1.49 with sigma of 0.02
 C31A-C27
 1.53 with sigma of 0.02
 C31-C27
 1.53 with sigma of 0.02
3. Rigid bond restraints
 C33, C33A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C32A, C32
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C31A, C31
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C31, C31A, C32, C32A, C33A, C33
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C33 \\sim C33A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C32A \\sim C32: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C31A \\sim C31: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C31 \\sim C31A \\sim C32 \\sim C32A \\sim C33A \\sim C33: within 1.7A with
sigma of 0.04 and sigma for terminal atoms of 0.08
Uiso(C33) = Uiso(C33A)
Uiso(C32A) = Uiso(C32)
Uiso(C31) = Uiso(C31A)
Uiso(C31) = Uiso(C31A) = Uiso(C32) = Uiso(C32A) = Uiso(C33A) = Uiso(C33)
5. Others
 Fixed Sof: C31(0.5) H31A(0.5) H31B(0.5) C32(0.5) H32(0.5) C33(0.5) H33A(0.5)
 H33B(0.5) C33A(0.5) H33C(0.5) H33D(0.5) C32A(0.5) H32A(0.5) C31A(0.5)
 H31C(0.5) H31D(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C31(H31A,H31B), C31A(H31C,H31D)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C9(H9), C11(H11), C13(H13), C15(H15), C16(H16), C19(H19),
 C20(H20), C21(H21), C22(H22), C23(H23), C26(H26), C28(H28), C32(H32), C34(H34),
  C36(H36), C38(H38), C39(H39), C42(H42), C43(H43), C44(H44), C45(H45),
 C46(H46), C47(H47), C50(H50), C53(H53), C56(H56), C59(H59), C32A(H32A)
6.c X=CH2 refined with riding coordinates:
 C10(H10A,H10B), C33(H33A,H33B), C33A(H33C,H33D)
6.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C24(H24A,H24B,H24C), C49(H49A,H49B,H49C), C51(H51A,H51B,
 H51C), C52(H52A,H52B,H52C), C54(H54A,H54B,H54C), C55(H55A,H55B,H55C), C57(H57A,
 H57B,H57C), C58(H58A,H58B,H58C), C60(H60A,H60B,H60C), C61(H61A,H61B,H61C),
 C48(H48A,H48B,H48C)
;
_olex2_submission_special_instructions 'No special instructions were received'