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_7221721
_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         'C38 H33 Co N6 O8, 2(C2 H3 N)'
_chemical_formula_sum            'C42 H39 Co N8 O8'
_chemical_formula_weight         842.74
_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   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2014-11-12
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_audit_update_record
;
2015-07-24 deposited with the CCDC.
2015-08-03 downloaded from the CCDC.
;
_cell_angle_alpha                77.797(2)
_cell_angle_beta                 79.842(2)
_cell_angle_gamma                72.698(3)
_cell_formula_units_Z            4
_cell_length_a                   12.6956(4)
_cell_length_b                   14.4449(4)
_cell_length_c                   22.4981(7)
_cell_measurement_temperature    100
_cell_volume                     3821.6(2)
_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 0.998
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0843
_diffrn_reflns_av_unetI/netI     0.1315
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            50559
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         2.187
_exptl_absorpt_coefficient_mu    0.516
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.740
_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    1.465
_exptl_crystal_description       plate
_exptl_crystal_F_000             1752
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.088
_refine_diff_density_min         -1.619
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1036
_refine_ls_number_reflns         17317
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.1450
_refine_ls_R_factor_gt           0.0746
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0454P)^2^+5.4720P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1315
_refine_ls_wR_factor_ref         0.1562
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10218
_reflns_number_total             17317
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce01294e2.cif
_cod_data_source_block           2014ncs0555z
_cod_depositor_comments
'Adding full bibliography for 7221715--7221724.cif.'
_cod_database_code               7221721
_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. Uiso/Uaniso restraints and constraints
Uiso(C72) = Uiso(C73) = Uiso(C74) = Uiso(C75) = Uiso(C76) = Uiso(C71A) =
Uiso(C73A) = Uiso(C74A) = Uiso(C75A) = Uiso(C76A) = Uiso(C71) = Uiso(C72A)
3. Others
 Fixed Sof: C71(0.5) C72(0.5) H72(0.5) C73(0.5) H73(0.5) C74(0.5) H74(0.5)
 C75(0.5) H75(0.5) C76(0.5) H76(0.5) C71A(0.5) H71A(0.5) C72A(0.5) C73A(0.5)
 H73A(0.5) C74A(0.5) H74A(0.5) C75A(0.5) H75A(0.5) C76A(0.5) H76A(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C8(H8), C15(H15), C16(H16), C17(H17), C18(H18),
 C19(H19), C22(H22), C23(H23), C24(H24), C27(H27), C34(H34), C35(H35), C36(H36),
  C37(H37), C38(H38), C41(H41), C42(H42), C43(H43), C46(H46), C53(H53),
 C54(H54), C55(H55), C56(H56), C57(H57), C60(H60), C61(H61), C62(H62), C65(H65),
  C72(H72), C73(H73), C74(H74), C75(H75), C76(H76), C71A(H71A), C73A(H73A),
 C74A(H74A), C75A(H75A), C76A(H76A)
4.b Fitted hexagon refined as free rotating group:
 C71(C72,C73,C74,C75,C76), C71A(C72A,C73A,C74A,C75A,C76A)
4.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C20(H20A,H20B,
 H20C), C32(H32A,H32B,H32C), C39(H39A,H39B,H39C), C50(H50A,H50B,H50C), C51(H51A,
 H51B,H51C), C58(H58A,H58B,H58C), C70(H70A,H70B,H70C), C82(H82A,H82B,H82C),
 C80(H80A,H80B,H80C), C84(H84A,H84B,H84C), C78(H78A,H78B,H78C)
;
_olex2_submission_special_instructions 'No special instructions were received'