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_7223519
_publ_section_title
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 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         'C118 H110 Dy2 N4 Ni2 O20, 5(C0.5 H Cl)'
_chemical_formula_sum            'C120.5 H115 Cl5 Dy2 N4 Ni2 O20'
_chemical_formula_weight         2558.83
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 100.127(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.1776(15)
_cell_length_b                   18.8940(11)
_cell_length_c                   27.8333(11)
_cell_measurement_temperature    173
_cell_volume                     11481.1(11)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      173.0
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.821
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.1362
_diffrn_reflns_laue_measured_fraction_full 0.987
_diffrn_reflns_laue_measured_fraction_max 0.821
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.821
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.316
_diffrn_reflns_theta_min         2.782
_exptl_absorpt_coefficient_mu    1.795
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.673
_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)
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.480
_exptl_crystal_description       prism
_exptl_crystal_F_000             5196
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.475
_refine_diff_density_min         -2.562
_refine_diff_density_rms         0.204
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     535
_refine_ls_number_reflns         12896
_refine_ls_number_restraints     264
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.1828
_refine_ls_R_factor_gt           0.1138
_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^)+(0.1504P)^2^+133.4705P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2803
_refine_ls_wR_factor_ref         0.3192
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7112
_reflns_number_total             12896
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce02109j2.cif
_cod_data_source_block           6_CCDC_1406222
_cod_depositor_comments
'Adding full bibliography for 7223506--7223525.cif.'
_cod_original_formula_sum        'C120.50 H115 Cl5 Dy2 N4 Ni2 O20'
_cod_database_code               7223519
_shelxl_version_number           2014-1
_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
 Cl3-C58
 1.78 with sigma of 0.02
 C25-C38
 1.24 with sigma of 0.02
 C8-C7
 1.24 with sigma of 0.02
 C15-C7
 1.45 with sigma of 0.02
 C50-C15
 1.53 with sigma of 0.02
 C39-C38
 1.31 with sigma of 0.02
 O10-H10
 0.87 with sigma of 0.01
 C61-H10
 1.927776 with sigma of 0.02
 Ni1-H10
 2.669128 with sigma of 0.02
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C25 \\sim C38: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
Uanis(C18) = Uanis(C19) = Uanis(C20) = Uanis(C21) = Uanis(C22) = Uanis(C23)
Uanis(C25) = Uanis(C38)
Uanis(C7) = Uanis(C15) = Uanis(C48) = Uanis(C49) = Uanis(C50) = Uanis(C51) =
Uanis(C52) = Uanis(C53) = Uanis(C54) = Uanis(C8)
Uanis(C2) = Uanis(C4AA) = Uanis(C4) = Uanis(C3) = Uanis(C5) = Uanis(C6) =
Uanis(C25) = Uanis(C38)
Uanis(C4) = Uanis(C3) = Uanis(C5) = Uanis(C25) = Uanis(C38) = Uanis(C39)
Uanis(C7) = Uanis(C8) = Uanis(C15) = Uanis(C48) = Uanis(C49) = Uanis(C50) =
Uanis(C51) = Uanis(C52) = Uanis(C53) = Uanis(C54)
5. Rigid body (RIGU) restrains
 C25, C38
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C7, C8, C15
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: Cl3(0.5) C58(0.25) H58A(0.25) H58B(0.25)
7.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C25(H25A,H25B), C31(H31A,H31B), C61(H61A,H61B), C58(H58A,
 H58B), C9(H9A,H9B)
7.b Me refined with riding coordinates:
 C0AA(H0AA,H0AB,H0AC), C24(H24A,H24B,H24C), C47(H47A,H47B,H47C), C62(H62A,H62B,
 H62C)
7.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C2AA(H2AA), C3AA(H3AA), C7(H7), C11(H11), C13(H13), C16(H16),
 C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C26(H26), C28(H28), C32(H32),
  C34(H34), C36(H36), C38(H38), C5AA(H5AA), C42(H42), C43(H43), C44(H44),
 C45(H45), C46(H46), C49(H49), C51(H51), C54(H54)
7.d Fitted hexagon refined as free rotating group:
 C2(C4AA,C4,C3,C5,C6)
7.e X=CH2 refined with riding coordinates:
 C8(H8A,H8B), C33(H33A,H33B), C39(H39A,H39B)
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_olex2_submission_special_instructions 'No special instructions were received'