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_7221723
_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 Cu4 N12 O14, 2(Cl O4), 6(C H4 O)'
_chemical_formula_sum            'C84 H102 Cl2 Cu4 N12 O28'
_chemical_formula_weight         2052.83
_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
_audit_creation_date             2015-02-20
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-07-24 deposited with the CCDC.
2015-08-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.9199(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.7809(3)
_cell_length_b                   19.3947(3)
_cell_length_c                   21.4148(2)
_cell_measurement_temperature    173
_cell_volume                     9782.8(2)
_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 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0295
_diffrn_reflns_av_unetI/netI     0.0451
_diffrn_reflns_laue_measured_fraction_full 0.991
_diffrn_reflns_laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            45640
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.373
_diffrn_reflns_theta_min         2.449
_exptl_absorpt_coefficient_mu    0.992
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.762
_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            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.394
_exptl_crystal_description       plate
_exptl_crystal_F_000             4256
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.851
_refine_diff_density_min         -0.758
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1156
_refine_ls_number_reflns         19849
_refine_ls_number_restraints     146
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0779
_refine_ls_R_factor_gt           0.0545
_refine_ls_shift/su_max          0.054
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0878P)^2^+5.6977P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1529
_refine_ls_wR_factor_ref         0.1682
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14428
_reflns_number_total             19849
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce01294e2.cif
_cod_data_source_block           exp_255
_cod_depositor_comments
'Adding full bibliography for 7221715--7221724.cif.'
_cod_database_code               7221723
_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, All O(H) groups
2. Restrained distances
 O0AA-Cl1
 1.41 with sigma of 0.02
 Cl1-O3AA
 1.41 with sigma of 0.02
 O2AA-Cl1
 1.41 with sigma of 0.02
 O1AA-Cl1
 1.41 with sigma of 0.02
 O0AA-Cl1
 1.41 with sigma of 0.02
 C3AA-O7AA
 1.43 with sigma of 0.02
 C1AA-O5AA
 1.43 with sigma of 0.02
 C0AA-O4AA
 1.43 with sigma of 0.02
 O0AA-Cl1
 1.41 with sigma of 0.02
 O0AB-Cl1
 1.41 with sigma of 0.02
 O1AB-Cl1
 1.41 with sigma of 0.02
 Cl1-O1AA
 1.41 with sigma of 0.02
 Cl1-O3AA
 1.41 with sigma of 0.02
 O3AB-Cl1
 1.41 with sigma of 0.02
 O2AB-Cl1
 1.41 with sigma of 0.02
 O2AA-Cl1
 1.41 with sigma of 0.02
 C2AA-O6AA
 1.43 with sigma of 0.02
3. Rigid bond restraints
 Cl2, O26, O27, O24, O25
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O17, H17A, C81, H81A, H81B, H81C
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O139, H139, C168, H16A, H16B, H16C
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Cl1, O0AA, O1AA, O2AA, O3AA
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Cl2 \\sim O26 \\sim O27 \\sim O24 \\sim O25: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08
O17 \\sim H17A \\sim C81 \\sim H81A \\sim H81B \\sim H81C: within 1.7A with
sigma of 0.04 and sigma for terminal atoms of 0.08
Cl1 \\sim O0AA \\sim O1AA \\sim O2AA \\sim O3AA: within 1.7A with sigma of 0.04
and sigma for terminal atoms of 0.08
5. Rigid body (RIGU) restrains
 Cl2, O26, O27, O24, O25
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O17, H17A, C81, H81A, H81B, H81C
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O139, H139, C168, H16A, H16B, H16C
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl1, O0AA
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl1, O0AA, O1AA, O2AA, O3AA
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: O0AA(0.5) O1AA(0.5) O2AA(0.5) O7AA(0.5) H7AA(0.5) O5AA(0.5)
 H5AA(0.5) O6AA(0.5) H6AA(0.5) O4AA(0.5) H4AA(0.5) C0AA(0.5) H0AA(0.5)
 H0AB(0.5) H0AC(0.5) C1AA(0.5) H1AA(0.5) H1AB(0.5) H1AC(0.5) C2AA(0.5)
 H2AA(0.5) H2AB(0.5) H2AC(0.5) C3AA(0.5) H3AA(0.5) H3AB(0.5) H3AC(0.5)
 O3AA(0.5) O3AB(0.5) O2AB(0.5) O0AB(0.5) O1AB(0.5)
7.a Riding coordinates:
 O139(H139), O7AA(H7AA), O5AA(H5AA), O6AA(H6AA), O4AA(H4AA)
7.b Me refined with riding coordinates:
 C69(H69A,H69B,H69C), C70(H70A,H70B,H70C), C77(H77A,H77B,H77C), C78(H78A,H78B,
 H78C), C20(H20A,H20B,H20C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C1(H1A,
 H1B,H1C), C13(H13A,H13B,H13C), C12(H12A,H12B,H12C), C58(H58A,H58B,H58C),
 C51(H51A,H51B,H51C), C50(H50A,H50B,H50C), C39(H39A,H39B,H39C), C81(H81A,H81B,
 H81C), C79(H79A,H79B,H79C), C95(H95A,H95B,H95C), C168(H16A,H16B,H16C),
 C0AA(H0AA,H0AB,H0AC), C1AA(H1AA,H1AB,H1AC), C2AA(H2AA,H2AB,H2AC), C3AA(H3AA,
 H3AB,H3AC)
7.c Aromatic/amide H refined with riding coordinates:
 C73(H73), C72(H72), C74(H74), C75(H75), C76(H76), C22(H22), C23(H23),
 C24(H24), C18(H18), C19(H19), C27(H27), C17(H17), C5(H5), C8(H8), C3(H3),
 C4(H4), C15(H15), C16(H16), C55(H55), C56(H56), C57(H57), C53(H53), C54(H54),
 C65(H65), C60(H60), C61(H61), C62(H62), C38(H38), C41(H41), C34(H34), C35(H35),
  C36(H36), C37(H37), C46(H46), C42(H42), C43(H43)
7.d Idealised tetrahedral OH refined as rotating group:
 O17(H17A), O15(H15A), O107(H107)
;
_olex2_submission_special_instructions 'No special instructions were received'