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_7223511
_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         'C88 H76 Co2 Dy2 N14 O34'
_chemical_formula_sum            'C88 H76 Co2 Dy2 N14 O34'
_chemical_formula_weight         2316.48
_chemical_name_systematic
;
 ?
;
_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   mixed
_atom_sites_solution_primary     iterative
_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                68.869(5)
_cell_angle_beta                 65.650(4)
_cell_angle_gamma                63.614(4)
_cell_formula_units_Z            1
_cell_length_a                   13.1490(9)
_cell_length_b                   13.6200(10)
_cell_length_c                   15.4701(11)
_cell_measurement_temperature    100
_cell_volume                     2207.1(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.992
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1033
_diffrn_reflns_av_unetI/netI     0.0580
_diffrn_reflns_laue_measured_fraction_full 0.996
_diffrn_reflns_laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            49522
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.628
_diffrn_reflns_theta_min         2.493
_exptl_absorpt_coefficient_mu    2.141
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.498
_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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.743
_exptl_crystal_description       block
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         4.512
_refine_diff_density_min         -2.629
_refine_diff_density_rms         0.267
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     621
_refine_ls_number_reflns         10202
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0859
_refine_ls_R_factor_gt           0.0745
_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^)+(0.1432P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1889
_refine_ls_wR_factor_ref         0.1971
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8620
_reflns_number_total             10202
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce02109j3.cif
_cod_data_source_block           18_CCDC_1406234
_cod_depositor_comments
'Adding full bibliography for 7223506--7223525.cif.'
_cod_database_code               7223511
_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
2. Restrained distances
 C17-C7
 1.3 with sigma of 0.02
 N3-C10
 1.53 with sigma of 0.02
 N3-C8
 1.53 with sigma of 0.02
3. Restrained planarity
 O8, N3, C6, C8, C10
 with sigma of 0.1
4. Rigid bond restraints
 C7, C17
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C7 \\sim C17: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
Uanis(C17) = Uanis(C7)
Uanis(C2) = Uanis(C17) = Uanis(C7)
6. Rigid body (RIGU) restrains
 C7, C17
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7.a Riding coordinates:
 C8(H8A,H8B,H8C)
7.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C12(H12A,H12B)
7.c Me refined with riding coordinates:
 C10(H10A,H10B,H10C)
7.d Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C15(H15), C17(H17), C20(H20), C23(H23), C24(H24), C25(H25),
 C39(H39), C44(H44), C45(H45), C47(H47), C52(H52), C65(H65), C69(H69), C71(H71),
  C75(H75), C78(H78)
7.e X=CH2 refined with riding coordinates:
 C7(H7A,H7B), C26(H26A,H26B)
7.f Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C29(H29A,H29B,H29C)
;
_shelx_res_checksum              45448
_olex2_submission_special_instructions 'No special instructions were received'