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_7221722
_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         'C58 H58 N9 Ni2 O10, 2(Cl0.5 O2), 2(C H4 O)'
_chemical_formula_sum            'C60 H66 Cl N9 Ni2 O16'
_chemical_formula_weight         1322.08
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2yc'
_space_group_name_H-M_alt        'I 1 2/c 1'
_symmetry_space_group_name_Hall  '-I 2yc'
_symmetry_space_group_name_H-M   'I 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2015-02-16
_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                 97.0327(8)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   27.0155(19)
_cell_length_b                   13.5650(9)
_cell_length_c                   36.028(3)
_cell_measurement_temperature    100
_cell_volume                     13103.7(17)
_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 0.982
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0721
_diffrn_reflns_av_unetI/netI     0.0460
_diffrn_reflns_laue_measured_fraction_full 0.988
_diffrn_reflns_laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            148453
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.472
_diffrn_reflns_theta_min         2.579
_exptl_absorpt_coefficient_mu    0.687
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.766
_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            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.340
_exptl_crystal_description       plate
_exptl_crystal_F_000             5520
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.801
_refine_diff_density_min         -0.685
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     767
_refine_ls_number_reflns         14748
_refine_ls_number_restraints     68
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0912
_refine_ls_R_factor_gt           0.0709
_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^)+(0.1380P)^2^+18.0900P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2040
_refine_ls_wR_factor_ref         0.2176
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11080
_reflns_number_total             14748
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce01294e2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 7221715--7221724.cif.'
_cod_original_cell_volume        13103.5(16)
_cod_database_code               7221722
_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
 O15-Cl1
 1.43 with sigma of 0.02
 Cl1-O16
 1.43 with sigma of 0.02
 Cl1-O18
 1.43 with sigma of 0.02
 Cl1-O17
 1.43 with sigma of 0.02
 O10-H10
 0.85 with sigma of 0.01
 O11-C59
 1.43 with sigma of 0.02
 N3-C14
 1.43 with sigma of 0.02
 C14A-N3
 1.43 with sigma of 0.02
 O17-Cl1
 1.43 with sigma of 0.02
 Cl1-O17A
 1.43 with sigma of 0.02
 O18A-Cl1
 1.43 with sigma of 0.02
 O18-Cl1
 1.43 with sigma of 0.02
 O16A-Cl1
 1.43 with sigma of 0.02
 O16-Cl1
 1.43 with sigma of 0.02
 Cl1-O15
 1.43 with sigma of 0.02
 Cl1-O15A
 1.43 with sigma of 0.02
 C58-H10
 1.872968 with sigma of 0.02
 Ni1-H10
 2.658743 with sigma of 0.02
3. Rigid bond restraints
 O17, Cl1, O15, O16, O18
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O12, C60, O11, C59
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Cl2, O13, O14
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
O17 \\sim Cl1 \\sim O15 \\sim O16 \\sim O18: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08
O12 \\sim C60 \\sim C59 \\sim O11: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
O13 \\sim Cl2 \\sim O14: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
5. Rigid body (RIGU) restrains
 O17, Cl1, O15, O16, O18
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O12, C60, C59, O11
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O13, Cl2, O14
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: C15(0.5) H15(0.5) C14(0.5) C19(0.5) H19(0.5) C18(0.5) H18(0.5)
 C17(0.5) H17(0.5) C16(0.5) H16(0.5) Cl1(0.5) O15(0.25) O16(0.25) O17(0.25)
 O18(0.25) C14A(0.5) C15A(0.5) H15A(0.5) C16A(0.5) H16A(0.5) C17A(0.5)
 H17A(0.5) C18A(0.5) H18A(0.5) C19A(0.5) H19A(0.5) O16A(0.25) O17A(0.25)
 O18A(0.25) O15A(0.25)
7.a Me refined with riding coordinates:
 C1(H1A,H1B,H1C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C20(H20A,H20B,
 H20C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C39(H39A,H39B,H39C), C50(H50A,
 H50B,H50C), C51(H51A,H51B,H51C), C58(H58A,H58B,H58C), C60(H60A,H60B,H60C)
7.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C8(H8), C15(H15), C19(H19), C18(H18), C17(H17),
 C16(H16), 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), C15A(H15A), C16A(H16A), C17A(H17A),
 C18A(H18A), C19A(H19A)
7.c Fitted hexagon refined as free rotating group:
 C15(C14,C19,C18,C17,C16), C14A(C15A,C16A,C17A,C18A,C19A)
7.d Tetrahedral OH refined with riding coordinates:
 O11(H11)
7.e Idealised Me refined as rotating group:
 C59(H59A,H59B,H59C)
7.f Idealised tetrahedral OH refined as rotating group:
 O12(H12)
;
_olex2_submission_special_instructions 'No special instructions were received'