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_7223521
_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         'C100 H78 Br6 Dy2 N4 Ni2 O20, 6(C2 H6 O)'
_chemical_formula_sum            'C112 H114 Br6 Dy2 N4 Ni2 O26'
_chemical_formula_weight         2848.01
_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             2015-01-10
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.06 svn.r3119 for OlexSys, GUI svn.r4979)
;
_audit_update_record
;
2015-11-15 deposited with the CCDC.
2015-12-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.444(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.4620(7)
_cell_length_b                   20.8069(7)
_cell_length_c                   27.3553(7)
_cell_measurement_temperature    173
_cell_volume                     11520.3(6)
_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_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.823
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0281
_diffrn_reflns_av_unetI/netI     0.0604
_diffrn_reflns_laue_measured_fraction_full 0.987
_diffrn_reflns_laue_measured_fraction_max 0.823
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            22076
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.823
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.133
_diffrn_reflns_theta_min         2.530
_exptl_absorpt_coefficient_mu    3.754
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.721
_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. 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    1.592
_exptl_crystal_description       block
_exptl_crystal_F_000             5472
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.772
_refine_diff_density_min         -3.539
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     652
_refine_ls_number_reflns         12759
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0746
_refine_ls_R_factor_gt           0.0501
_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^)+(0.0805P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1310
_refine_ls_wR_factor_ref         0.1431
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9196
_reflns_number_total             12759
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce02109j2.cif
_cod_data_source_block           8_CCDC_1406224
_cod_depositor_comments
'Adding full bibliography for 7223506--7223525.cif.'
_cod_original_cell_volume        11520.3(7)
_cod_database_code               7223521
_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
 O11-C49
 1.43 with sigma of 0.02
 O12-C51
 1.43 with sigma of 0.02
 C51-C52
 1.54 with sigma of 0.02
 C50-C49
 1.54 with sigma of 0.02
 O10-H10
 0.87 with sigma of 0.01
 C4-H10
 1.877518 with sigma of 0.02
 Ni1-H10
 2.650389 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C1) = Uanis(C4) = Uanis(O10)
4.a Secondary CH2 refined with riding coordinates:
 C49(H49A,H49B), C51(H51A,H51B)
4.b Me refined with riding coordinates:
 C21(H21A,H21B,H21C), C41(H41A,H41B,H41C), C50(H50A,H50B,H50C), C52(H52A,H52B,
 H52C), C1(H1A,H1B,H1C)
4.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C8(H8), C10(H10A), C12(H12), C13(H13), C16(H16), C17(H17),
 C18(H18), C19(H19), C20(H20), C23(H23), C25(H25), C28(H28), C30(H30), C32(H32),
  C33(H33), C36(H36), C37(H37), C38(H38), C39(H39), C40(H40), C43(H43),
 C45(H45), C48(H48), C4(H4)
4.d Idealised Me refined as rotating group:
 C0AA(H0AA,H0AB,H0AC)
4.e Idealised tetrahedral OH refined as rotating group:
 O11(H11), O12(H12A)
;
_shelx_res_checksum              77579
_olex2_submission_special_instructions 'No special instructions were received'