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_7221724
_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         'C36 H50 Cl2 Co4 N2 O14'
_chemical_formula_sum            'C36 H50 Cl2 Co4 N2 O14'
_chemical_formula_weight         1041.40
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2015-03-03
_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                90
_cell_angle_beta                 101.320(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.7862(5)
_cell_length_b                   21.7148(8)
_cell_length_c                   16.7640(6)
_cell_measurement_reflns_used    6334
_cell_measurement_temperature    173
_cell_measurement_theta_max      28.9300
_cell_measurement_theta_min      3.6550
_cell_volume                     4207.0(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
;
_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    'ShelXT (Sheldrick, 2008)'
_diffrn_ambient_temperature      173
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1033
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega  -73.00  -41.00   1.0000   86.4250
omega____ theta____ kappa____ phi______ frames
    -      -16.1295 -178.0000 -120.0000 32

  2 omega  -83.00   -2.00   1.0000   86.4250
omega____ theta____ kappa____ phi______ frames
    -      -16.1295  -57.0000   30.0000 81

  3 omega  -43.00   51.00   1.0000   86.4250
omega____ theta____ kappa____ phi______ frames
    -      -16.1295   77.0000  150.0000 94

  4 omega   -4.00   21.00   1.0000   86.4250
omega____ theta____ kappa____ phi______ frames
    -       16.7545  -99.0000 -150.0000 25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0280646000
_diffrn_orient_matrix_UB_12      -0.0184960000
_diffrn_orient_matrix_UB_13      -0.0328983000
_diffrn_orient_matrix_UB_21      0.0007681000
_diffrn_orient_matrix_UB_22      0.0250763000
_diffrn_orient_matrix_UB_23      -0.0270607000
_diffrn_orient_matrix_UB_31      0.0545150000
_diffrn_orient_matrix_UB_32      -0.0098795000
_diffrn_orient_matrix_UB_33      -0.0069783000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0378
_diffrn_reflns_av_unetI/netI     0.0495
_diffrn_reflns_laue_measured_fraction_full 0.997
_diffrn_reflns_laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            19374
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.321
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.743
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64759
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
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    1.644
_exptl_crystal_description       block
_exptl_crystal_F_000             2136
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.442
_refine_diff_density_min         -0.381
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     536
_refine_ls_number_reflns         8574
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0517
_refine_ls_R_factor_gt           0.0372
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0370P)^2^+1.6650P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0850
_refine_ls_wR_factor_ref         0.0938
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6869
_reflns_number_total             8574
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce01294e2.cif
_cod_data_source_block           kg0325022015
_cod_depositor_comments
'Adding full bibliography for 7221715--7221724.cif.'
_cod_database_code               7221724
_chemical_oxdiff_formula         Co4C60H80O12N8
_reflns_odcompleteness_completeness 99.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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
 O00F-H00F
 0.85 with sigma of 0.01
 O00I-H00I
 0.85 with sigma of 0.01
 O11-H11
 0.85 with sigma of 0.01
 O12-H12
 0.85 with sigma of 0.01
 C01D-H00F
 1.914474 with sigma of 0.02
 Co1-H00F
 2.562249 with sigma of 0.02
 C01F-H00I
 1.90004 with sigma of 0.02
 Co4-H00I
 2.582277 with sigma of 0.02
 C33-H11
 1.894923 with sigma of 0.02
 Co2-H11
 2.701342 with sigma of 0.02
 C34-H12
 1.894754 with sigma of 0.02
 Co3-H12
 2.68658 with sigma of 0.02
3.a Me refined with riding coordinates:
 C1(H1A,H1B,H1C), C01D(H01A,H01B,H01C), C15(H15A,H15B,H15C), C29(H29A,H29B,
 H29C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C33(H33A,
 H33B,H33C), C34(H34A,H34B,H34C)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C8(H8), C10(H10), C11(H11A), C12(H12A), C13(H13),
 C17(H17), C18(H18), C19(H19), C22(H22), C24(H24), C25(H25), C26(H26), C27(H27)
3.c Idealised Me refined as rotating group:
 C01F(H01D,H01E,H01F)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'