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_7223508
_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         'C84 H88 Dy2 N4 Ni2 O18, 2(Cl O4), 4(C2 H6 O)'
_chemical_formula_sum            'C92 H112 Cl2 Dy2 N4 Ni2 O30'
_chemical_formula_weight         2267.18
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-05-07
_audit_creation_method
;
Olex2 1.2
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_audit_update_record
;
2015-11-15 deposited with the CCDC.
2015-12-17 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 98.464(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.19560(19)
_cell_length_b                   19.3817(6)
_cell_length_c                   20.2019(7)
_cell_measurement_reflns_used    11651
_cell_measurement_temperature    173
_cell_measurement_theta_max      29.0330
_cell_measurement_theta_min      2.9540
_cell_volume                     4723.1(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
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SUPERFLIP, J. Appl. Cryst. (2007) 40, 786-790'
_diffrn_ambient_temperature      173
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1033
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9986
_diffrn_measured_fraction_theta_max 0.8662
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0327873000
_diffrn_orient_matrix_UB_12      -0.0058534000
_diffrn_orient_matrix_UB_13      -0.0315424000
_diffrn_orient_matrix_UB_21      -0.0485542000
_diffrn_orient_matrix_UB_22      0.0079301000
_diffrn_orient_matrix_UB_23      0.0140527000
_diffrn_orient_matrix_UB_31      0.0054549000
_diffrn_orient_matrix_UB_32      0.0352559000
_diffrn_orient_matrix_UB_33      -0.0084239000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0320
_diffrn_reflns_av_unetI/netI     0.0412
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            29019
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         29.16
_diffrn_reflns_theta_min         2.66
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.095
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77013
_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    1.594
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2308
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.184
_refine_diff_density_min         -0.542
_refine_diff_density_rms         0.100
_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     613
_refine_ls_number_reflns         11050
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0451
_refine_ls_R_factor_gt           0.0322
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0254P)^2^+6.0180P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0687
_refine_ls_wR_factor_ref         0.0755
_reflns_number_gt                9123
_reflns_number_total             11050
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ce02109j3.cif
_cod_data_source_block           15_CCDC_1406231
_cod_depositor_comments
'Adding full bibliography for 7223506--7223525.cif.'
_cod_database_code               7223508
_chemical_oxdiff_formula         Ni4Dy2C80H80N10O30
_reflns_odcompleteness_completeness 99.86
_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, All O(H) groups
2. Restrained distances
 O8-H8
 0.85 with sigma of 0.01
 O7-H7
 0.85 with sigma of 0.01
 O17-H17A
 0.85 with sigma of 0.01
 C41-H8
 1.915567 with sigma of 0.02
 Ni1-H8
 2.879742 with sigma of 0.02
 C39-H7
 1.904837 with sigma of 0.02
 Dy1-H7
 2.933457 with sigma of 0.02
 C37-H17A
 1.888896 with sigma of 0.02
 Dy1-H17A
 2.917467 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C39(H39A,H39B), C37(H37A,H37B), C41(H41A,H41B), C43(H43A,H43B), C45(H45A,H45B)
3.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C17(H17), C15(H15), C30(H30), C21(H21), C33(H33), C22(H22),
 C26(H26), C13(H13), C12(H12), C5(H5), C23(H23), C35(H35), C14(H14), C4(H4),
 C8(H8A), C28(H28), C31(H31), C32(H32), C3(H3)
3.c Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C42(H42A,H42B,H42C), C38(H38A,H38B,H38C), C1(H1A,H1B,
 H1C), C40(H40A,H40B,H40C), C44(H44A,H44B,H44C), C46(H46A,H46B,H46C)
3.d Idealised tetrahedral OH refined as rotating group:
 O9(H9), O10(H10A)
;
_shelx_res_checksum              49787