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_7223517
_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         'C28 H20 Co N4 O10, 2(C H4 O), C6 H16 N'
_chemical_formula_sum            'C36 H44 Co N5 O12'
_chemical_formula_weight         797.69
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2015-01-09
_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                 108.353(8)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.8624(5)
_cell_length_b                   17.0300(4)
_cell_length_c                   25.6461(18)
_cell_measurement_temperature    100
_cell_volume                     7819.2(7)
_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 0.988
_diffrn_measured_fraction_theta_max 0.974
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0518
_diffrn_reflns_av_unetI/netI     0.0621
_diffrn_reflns_laue_measured_fraction_full 0.988
_diffrn_reflns_laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            61781
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.481
_diffrn_reflns_theta_min         3.052
_exptl_absorpt_coefficient_mu    0.505
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.800
_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    1.355
_exptl_crystal_description       plate
_exptl_crystal_F_000             3344
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.400
_refine_diff_density_min         -1.246
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     955
_refine_ls_number_reflns         17458
_refine_ls_number_restraints     93
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.1216
_refine_ls_R_factor_gt           0.0855
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1081P)^2^+18.2835P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2181
_refine_ls_wR_factor_ref         0.2379
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11644
_reflns_number_total             17458
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce02109j2.cif
_cod_data_source_block           4_CCDC_1406220
_cod_depositor_comments
'Adding full bibliography for 7223506--7223525.cif.'
_cod_database_code               7223517
_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, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 C18-N206
 1.42 with sigma of 0.02
 N3-C18
 1.42 with sigma of 0.02
 N29-C162
 1.51 with sigma of 0.02
 C8-N1
 1.51 with sigma of 0.02
 N1-C1
 1.51 with sigma of 0.02
 C6-C1
 1.51 with sigma of 0.02
 C2-N1
 1.51 with sigma of 0.02
 C4-C2
 1.51 with sigma of 0.02
 C5-C8
 1.51 with sigma of 0.02
3. Rigid bond restraints
 N1, C1, C2, C4, C5, C6, C8
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
N1 \\sim C1 \\sim C2 \\sim C4 \\sim C5 \\sim C6 \\sim C8: within 1.7A with
sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C19) = Uanis(C18) = Uanis(C17) = Uanis(C16) = Uanis(C21) = Uanis(C20)
5. Rigid body (RIGU) restrains
 N1, C1, C2, C4, C5, C6, C8
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: O5(0.5) O78(0.5) O78A(0.5) O104(0.5) N3(0.5) N206(0.5)
7.a Riding coordinates:
 C2AA(H2AA,H2AB,H2AC), C8(H8A,H8B)
7.b Ternary CH refined with riding coordinates:
 N1(H1), N29(H29)
7.c Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C68(H68A,H68B), C125(H12A,H12B), C162(H16A,H16B)
7.d Me refined with riding coordinates:
 C0AA(H0AA,H0AB,H0AC), C121(H12D,H12E,H12F)
7.e Aromatic/amide H refined with riding coordinates:
 C31(H31), C33(H33), C36(H36), C38(H38), C39(H39), C40(H40), C41(H41),
 C45(H45), C47(H47), C50(H50), C52(H52), C53(H53), C54(H54), C55(H55), C3(H3),
 C5AA(H5AA), C7AA(H7AA), C10(H10), C11(H11), C12(H12), C13(H13), C17(H17),
 C19(H19), C22(H22), C24(H24), C25(H25), C26(H26), C27(H27)
7.f Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C43(H43A,H43B,H43C), C15(H15A,H15B,H15C), C58(H58A,H58B,
 H58C), C59(H59A,H59B,H59C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C),
 C6AA(H6AA,H6AB,H6AC), C210(H21A,H21B,H21C), C226(H22A,H22B,H22C)
7.g Idealised tetrahedral OH refined as rotating group:
 O82(H82), O74(H74), O12(H12C), O14(H14)
;
_shelx_res_checksum              11322
_olex2_submission_special_instructions 'No special instructions were received'