Cobalt(ii/iii), nickel(ii) and copper(ii) coordination clusters employing a monoanionic Schiff base ligand: synthetic, topological and computational mechanistic aspects
Loukopoulos, Edward; Berkoff, Benjamin; Griffiths, Kieran; Keeble, Victoria; Dokorou, Vassiliki N.; Tsipis, Athanassios C.; Escuer, Albert; Kostakis, George E.; CrystEngComm 17 (2015) 6753–; doi:10.1039/C5CE01294E

data_7221718
_publ_section_title
;
 Cobalt(ii/iii), nickel(ii) and copper(ii) coordination clusters employing
 a monoanionic Schiff base ligand: synthetic, topological and
 computational mechanistic aspects
;
_journal_issue                   35
_journal_name_full               CrystEngComm
_journal_page_first              6753
_journal_paper_doi               10.1039/C5CE01294E
_journal_volume                  17
_journal_year                    2015
_chemical_formula_moiety         'C78 H78 Co4 N12 O14, 2(Cl O4)'
_chemical_formula_sum            'C78 H78 Cl2 Co4 N12 O22'
_chemical_formula_weight         1842.14
_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   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2014-05-19
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_audit_update_record
;
2015-07-24 deposited with the CCDC.
2015-08-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.306(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.5066(6)
_cell_length_b                   12.3910(3)
_cell_length_c                   29.062(2)
_cell_measurement_temperature    150
_cell_volume                     7988.9(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      150
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  2014ncs0285_info
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0793
_diffrn_reflns_av_unetI/netI     0.0695
_diffrn_reflns_laue_measured_fraction_full 0.987
_diffrn_reflns_laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            90215
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         3.081
_exptl_absorpt_coefficient_mu    0.966
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.395
_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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.532
_exptl_crystal_description       plate
_exptl_crystal_F_000             3792
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.790
_refine_diff_density_min         -1.696
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     992
_refine_ls_number_reflns         18111
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0995
_refine_ls_R_factor_gt           0.0690
_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^)+(0.1221P)^2^+6.6064P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1874
_refine_ls_wR_factor_ref         0.2090
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12528
_reflns_number_total             18111
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce01294e2.cif
_cod_data_source_block           2014ncs0285
_cod_depositor_comments
'Adding full bibliography for 7221715--7221724.cif.'
_cod_original_cell_volume        7988.8(7)
_cod_database_code               7221718
_shelxl_version_number           2014-1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C68, C69, C70, C71, C72, C73
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C68 \\sim C69 \\sim C70 \\sim C71 \\sim C72 \\sim C73: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08
Uiso(C30) = Uiso(C31) = Uiso(C32) = Uiso(C33) = Uiso(C34) = Uiso(C35) =
Uiso(C79) = Uiso(C80) = Uiso(C81) = Uiso(C82) = Uiso(C83) = Uiso(C84)
Uanis(C68) = Uanis(C69) = Uanis(C70) = Uanis(C71) = Uanis(C72) = Uanis(C73)
4. Others
 Fixed Sof: C35(0.5) H35(0.5) C34(0.5) H34(0.5) C33(0.5) H33(0.5) C32(0.5)
 H32(0.5) C31(0.5) H31(0.5) C30(0.5) C79(0.5) C84(0.5) H84(0.5) C83(0.5)
 H83(0.5) C82(0.5) H82(0.5) C81(0.5) H81(0.5) C80(0.5) H80(0.5) O21(0.5)
 O22(0.5) O23(0.5) O24(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C8(H8), C12(H12), C13(H13), C14(H14), C15(H15),
 C16(H16), C24(H24), C25(H25), C26(H26), C27(H27), C35(H35), C34(H34), C33(H33),
  C32(H32), C31(H31), C41(H41), C42(H42), C43(H43), C46(H46), C49(H49),
 C50(H50), C51(H51), C52(H52), C53(H53), C60(H60), C61(H61), C62(H62), C65(H65),
  C69(H69), C70(H70), C71(H71), C72(H72), C73(H73), C84(H84), C83(H83),
 C82(H82), C81(H81), C80(H80)
5.b Fitted hexagon refined as free rotating group:
 C35(C34,C33,C32,C31,C30), C68(C69,C70,C71,C72,C73), C79(C84,C83,C82,C81,C80)
5.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C17(H17A,H17B,H17C), C19(H19A,H19B,H19C), C20(H20A,H20B,
 H20C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C39(H39A,H39B,H39C), C54(H54A,
 H54B,H54C), C56(H56A,H56B,H56C), C58(H58A,H58B,H58C), C74(H74A,H74B,H74C),
 C76(H76A,H76B,H76C), C77(H77A,H77B,H77C), C78(H78A,H78B,H78C)
;