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_7221719
_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         'C76 H76 Co4 N12 O20'
_chemical_formula_sum            'C76 H76 Co4 N12 O20'
_chemical_formula_weight         1713.20
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a'
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2015-02-06
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.0627(5)
_cell_length_b                   15.0627(5)
_cell_length_c                   33.6307(16)
_cell_measurement_reflns_used    3902
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.5280
_cell_measurement_theta_min      3.3050
_cell_volume                     7630.3(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_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_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1033
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.855
_diffrn_measurement_details
;
  1 omega  -42.00   45.00   1.0000  200.2800
omega____ theta____ kappa____ phi______ frames
    -      -18.0128   19.0000   30.0000 87

  2 omega  -24.00   11.00   1.0000  200.2800
omega____ theta____ kappa____ phi______ frames
    -      -18.0128  -19.0000  120.0000 35
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0216423000
_diffrn_orient_matrix_UB_12      -0.0359059000
_diffrn_orient_matrix_UB_13      0.0096311000
_diffrn_orient_matrix_UB_21      0.0127397000
_diffrn_orient_matrix_UB_22      -0.0174281000
_diffrn_orient_matrix_UB_23      -0.0187348000
_diffrn_orient_matrix_UB_31      0.0397046000
_diffrn_orient_matrix_UB_32      0.0252593000
_diffrn_orient_matrix_UB_33      0.0008312000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0247
_diffrn_reflns_av_unetI/netI     0.0330
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.855
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            9400
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.855
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.106
_diffrn_reflns_theta_min         2.964
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.936
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76909
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
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    1.491
_exptl_crystal_description       block
_exptl_crystal_F_000             3536
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.355
_refine_diff_density_min         -0.407
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     256
_refine_ls_number_reflns         4382
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0652
_refine_ls_R_factor_gt           0.0485
_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^)+(0.0873P)^2^+5.6638P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1378
_refine_ls_wR_factor_ref         0.1500
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3427
_reflns_number_total             4382
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce01294e2.cif
_cod_data_source_block           vnca
_cod_depositor_comments
'Adding full bibliography for 7221715--7221724.cif.'
_cod_original_cell_volume        7630.3(6)
_cod_database_code               7221719
_shelxl_version_number           2014-1
_chemical_oxdiff_formula         Co4C72H72N3O12
_reflns_odcompleteness_completeness 99.72
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H5A(0.068) H5B(0.068) H1A(0.094) H1B(0.094) H1C(0.094) H3(0.059)
 H4(0.057) H5(0.049) H8(0.038) H13(0.05) H14(0.062) H15(0.072) H16(0.077)
 H17(0.065) H18A(0.067) H18B(0.067) H18C(0.067) H19A(0.036) H19B(0.036)
 Fixed X: H5A(0.5408) H5B(0.4657) H1A(0.0668) H1B(0.0266) H1C(0.0826)
 H3(0.0664) H4(0.1237) H5(0.2736) H8(0.4159) H13(0.6653) H14(0.7412)
 H15(0.8179) H16(0.8154) H17(0.7372) H18A(0.8008) H18B(0.8104) H18C(0.7977)
 H19A(0.6649) H19B(0.701)
 Fixed Y: H5A(0.5254) H5B(0.4881) H1A(0.6989) H1B(0.6369) H1C(0.7234)
 H3(0.5632) H4(0.5199) H5(0.5297) H8(0.571) H13(0.5556) H14(0.5747) H15(0.7058)
 H16(0.8207) H17(0.8043) H18A(0.7507) H18B(0.6533) H18C(0.6656) H19A(0.6145)
 H19B(0.7131)
 Fixed Z: H5A(0.6221) H5B(0.6046) H1A(0.6295) H1B(0.5953) H1C(0.5837)
 H3(0.541) H4(0.4793) H5(0.4674) H8(0.4835) H13(0.4051) H14(0.345) H15(0.3324)
 H16(0.3782) H17(0.438) H18A(0.5031) H18B(0.4846) H18C(0.5315) H19A(0.5816)
 H19B(0.5744)
;
_olex2_submission_special_instructions 'No special instructions were received'