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_7223523
_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         'C102 H110 Dy2 N10 Ni2 O18, 2(Cl O4)'
_chemical_formula_sum            'C102 H110 Cl2 Dy2 N10 Ni2 O26'
_chemical_formula_weight         2405.31
_chemical_name_systematic
;
 ?
;
_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
_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                90
_cell_angle_beta                 96.747(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.8855(6)
_cell_length_b                   17.2105(11)
_cell_length_c                   20.5903(11)
_cell_measurement_reflns_used    9830
_cell_measurement_temperature    173
_cell_measurement_theta_max      28.7690
_cell_measurement_theta_min      2.9240
_cell_volume                     5590.3(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 0.998
_diffrn_measured_fraction_theta_max 0.868
_diffrn_measurement_details
;
  1 omega  -38.00   50.00   1.0000    2.5400
omega____ theta____ kappa____ phi______ frames
    -      -18.1690   57.0000  -30.0000 88

  2 omega  -32.00   43.00   1.0000    2.5400
omega____ theta____ kappa____ phi______ frames
    -      -18.1690   57.0000   90.0000 75

  3 omega   26.00   51.00   1.0000    2.5400
omega____ theta____ kappa____ phi______ frames
    -      -18.1690   57.0000  150.0000 25

  4 omega  -36.00   10.00   1.0000    2.5400
omega____ theta____ kappa____ phi______ frames
    -      -18.1690   57.0000  150.0000 46

  5 omega  -89.00  -53.00   1.0000    2.5400
omega____ theta____ kappa____ phi______ frames
    -      -18.1690  178.0000  120.0000 36

  6 omega  -80.00  -43.00   1.0000    2.5400
omega____ theta____ kappa____ phi______ frames
    -      -18.1690 -178.0000  -60.0000 37
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0073669000
_diffrn_orient_matrix_UB_12      0.0271064000
_diffrn_orient_matrix_UB_13      -0.0259709000
_diffrn_orient_matrix_UB_21      0.0372428000
_diffrn_orient_matrix_UB_22      -0.0128569000
_diffrn_orient_matrix_UB_23      -0.0125947000
_diffrn_orient_matrix_UB_31      -0.0240314000
_diffrn_orient_matrix_UB_32      -0.0282308000
_diffrn_orient_matrix_UB_33      -0.0191528000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_unetI/netI     0.0495
_diffrn_reflns_laue_measured_fraction_full 0.998
_diffrn_reflns_laue_measured_fraction_max 0.868
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            13138
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.868
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.188
_diffrn_reflns_theta_min         2.536
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.774
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61710
_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    1.429
_exptl_crystal_F_000             2444
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.236
_refine_diff_density_min         -1.236
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     664
_refine_ls_number_reflns         13129
_refine_ls_number_restraints     446
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0708
_refine_ls_R_factor_gt           0.0464
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0578P)^2^+3.7604P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1115
_refine_ls_wR_factor_ref         0.1220
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9655
_reflns_number_total             13129
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce02109j2.cif
_cod_data_source_block           10_CCDC_1406226
_cod_depositor_comments
'Adding full bibliography for 7223506--7223525.cif.'
_cod_database_code               7223523
_shelxl_version_number           2014-1
_chemical_oxdiff_formula         Ni2Dy2C120H150N14O30
_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
2. Restrained distances
 O13-Cl1
 1.43 with sigma of 0.02
 O11-Cl1
 1.43 with sigma of 0.02
 O14-Cl1
 1.43 with sigma of 0.02
 O12-Cl1
 1.43 with sigma of 0.02
 Cl1-O15
 1.43 with sigma of 0.02
 C43-N3
 1.32 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
4. Others
 Fixed Sof: O13(0.5) O12(0.5) O11(0.5) O15(0.5) O11A(0.5) O13A(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C29(H29A,H29B)
5.b Aromatic/amide H refined with riding coordinates:
 C30(H30), C5(H5), C39(H39), C37(H37), C3(H3), C20(H20), C9(H9), C13(H13),
 C36(H36), C17(H17), C11(H11), C34(H34), C26(H26), C16(H16), C38(H38), C32(H32),
  C15(H15), C46(H46), C24(H24), C41(H41), C49(H49), C43(H43), C18(H18)
5.c X=CH2 refined with riding coordinates:
 C10(H10A,H10B), C31(H31A,H31B)
5.d Idealised Me refined as rotating group:
 C47(H47A,H47B,H47C), C22(H22A,H22B,H22C), C51(H51A,H51B,H51C), C50(H50A,H50B,
 H50C), C48(H48A,H48B,H48C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C1(H1A,
 H1B,H1C)
;
_olex2_submission_special_instructions 'No special instructions were received'