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_7221715
_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 H36 Co N6 O6, 5(C2 H3 N)'
_chemical_formula_sum            'C48 H51 Co N11 O6'
_chemical_formula_weight         936.92
_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     direct
_audit_creation_date             2015-03-13
_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                88.395(10)
_cell_angle_beta                 88.618(9)
_cell_angle_gamma                89.946(10)
_cell_formula_units_Z            2
_cell_length_a                   12.5772(15)
_cell_length_b                   13.5174(19)
_cell_length_c                   13.8758(14)
_cell_measurement_temperature    173
_cell_volume                     2357.4(5)
_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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      173.0
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.807
_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     0.0618
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.807
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14989
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.807
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.373
_diffrn_reflns_theta_min         3.391
_exptl_absorpt_coefficient_mu    0.425
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.647
_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    1.320
_exptl_crystal_description       block
_exptl_crystal_F_000             982
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.336
_refine_diff_density_min         -0.408
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     606
_refine_ls_number_reflns         10479
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0723
_refine_ls_R_factor_gt           0.0525
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0526P)^2^+0.9522P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1216
_refine_ls_wR_factor_ref         0.1349
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8089
_reflns_number_total             10479
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce01294e2.cif
_cod_data_source_block           w11d13bb
_cod_depositor_comments
'Adding full bibliography for 7221715--7221724.cif.'
_cod_database_code               7221715
_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.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)
2.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C20(H20A,H20B,
 H20C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C42(H42A,H42B,H42C), C40(H40A,
 H40B,H40C), C44(H44A,H44B,H44C), C46(H46A,H46B,H46C), C48(H48A,H48B,H48C)
;
_shelx_res_checksum              38767
_olex2_submission_special_instructions 'No special instructions were received'