Isoskeletal Schiff base polynuclear coordination clusters: synthetic and theoretical aspects
Griffiths, Kieran; Dokorou, Vassiliki N.; Spencer, John; Abdul-Sada, Alaa; Vargas, Alfredo; Kostakis, George E.; CrystEngComm 18 (2016) 704–; doi:10.1039/C5CE02109J

data_7223518
_publ_section_title
;
 Isoskeletal Schiff base polynuclear coordination clusters: synthetic and
 theoretical aspects
;
_journal_issue                   5
_journal_name_full               CrystEngComm
_journal_page_first              704
_journal_paper_doi               10.1039/C5CE02109J
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         'C36 H24 Br2 Co N2 O6, C6 H16 N, 3(C H4 O)'
_chemical_formula_sum            'C45 H52 Br2 Co N3 O9'
_chemical_formula_weight         997.64
_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
_audit_creation_date             2015-11-14
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2015-11-15 deposited with the CCDC.
2015-12-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.616(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.0590(8)
_cell_length_b                   22.7258(11)
_cell_length_c                   15.4472(13)
_cell_measurement_reflns_used    3201
_cell_measurement_temperature    173
_cell_measurement_theta_max      26.8380
_cell_measurement_theta_min      2.8660
_cell_volume                     4318.3(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      173
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1033
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.955
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_details
;
  1 omega  -87.00    3.00   1.0000  150.4700
omega____ theta____ kappa____ phi______ frames
    -      -18.0128  -57.0000   30.0000 90

  2 omega  -44.00   31.00   1.0000  150.4700
omega____ theta____ kappa____ phi______ frames
    -      -18.0128   77.0000  150.0000 75
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0287118000
_diffrn_orient_matrix_UB_12      0.0166250000
_diffrn_orient_matrix_UB_13      -0.0395587000
_diffrn_orient_matrix_UB_21      -0.0254367000
_diffrn_orient_matrix_UB_22      -0.0260680000
_diffrn_orient_matrix_UB_23      -0.0223367000
_diffrn_orient_matrix_UB_31      -0.0430939000
_diffrn_orient_matrix_UB_32      0.0043186000
_diffrn_orient_matrix_UB_33      0.0176033000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0365
_diffrn_reflns_av_unetI/netI     0.0800
_diffrn_reflns_Laue_measured_fraction_full 0.955
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13404
_diffrn_reflns_point_group_measured_fraction_full 0.955
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         2.440
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.307
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71537
_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    1.535
_exptl_crystal_description       plate
_exptl_crystal_F_000             2048
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.769
_refine_diff_density_min         -0.815
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     543
_refine_ls_number_reflns         8410
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.1023
_refine_ls_R_factor_gt           0.0590
_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^)+(0.0486P)^2^+4.6912P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1182
_refine_ls_wR_factor_ref         0.1402
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5589
_reflns_number_total             8410
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce02109j2.cif
_cod_data_source_block           5_CCDC_1406221
_cod_depositor_comments
'Adding full bibliography for 7223506--7223525.cif.'
_cod_database_code               7223518
_shelxl_version_number           2014-1
_chemical_oxdiff_formula         Co4C80H88N8O32
_reflns_odcompleteness_completeness 95.18
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H45A,H45B,H45C} of C45, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H) groups, {H1A,H1B,H1C} of C1, {H19A,H19B,H19C} of C19, {H40A,H40B,
  H40C} of C40, {H38A,H38B,H38C} of C38, {H44A,H44B,H44C} of C44, {H43A,H43B,
  H43C} of C43, {H42A,H42B,H42C} of C42
2.a Riding coordinates:
 C1(H1A,H1B,H1C), C19(H19A,H19B,H19C), C38(H38A,H38B,H38C), C40(H40A,H40B,
 H40C), C42(H42A,H42B,H42C), O9(H9), C43(H43A,H43B,H43C), C45(H45A,H45B,H45C)
2.b Ternary CH refined with riding coordinates:
 N3(H3A)
2.c Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B), C39(H39A,H39B), C41(H41A,H41B)
2.d Me refined with riding coordinates:
 C44(H44A,H44B,H44C)
2.e Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C8(H8), C10(H10), C12(H12), C13(H13), C14(H14), C15(H15),
 C17(H17), C21(H21), C23(H23), C26(H26), C28(H28), C30(H30), C31(H31), C32(H32),
  C33(H33), C35(H35)
2.f Idealised tetrahedral OH refined as rotating group:
 O7(H7), O8(H8A)
;
_olex2_submission_special_instructions 'No special instructions were received'