Polynuclear ampyrone based 3d coordination clusters
Sampani, Stavroula I.; Loukopoulos, Edward; Azam, Mohammad; Griffiths, Kieran; Abdul-Sada, Alaa; Tizzard, Graham; Coles, Simon; Escuer, Albert; Tsipis, Athanassios; Kostakis, George E.; CrystEngComm 20 (2018) 1411–; doi:10.1039/C7CE02093G

data_7230052
_publ_section_title
;
 Polynuclear ampyrone based 3d coordination clusters
;
_journal_issue                   10
_journal_name_full               CrystEngComm
_journal_page_first              1411
_journal_paper_doi               10.1039/C7CE02093G
_journal_volume                  20
_journal_year                    2018
_chemical_formula_moiety         'C36 H32 N6 Ni O4, 3(C2 H3 N)'
_chemical_formula_sum            'C42 H41 N9 Ni O4'
_chemical_formula_weight         794.55
_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   geom
_audit_creation_date             2017-09-19
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2017-12-04 deposited with the CCDC.
2018-01-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.3925(19)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.9150(2)
_cell_length_b                   13.7467(2)
_cell_length_c                   20.8267(4)
_cell_measurement_reflns_used    4893
_cell_measurement_temperature    173
_cell_measurement_theta_max      70.4570
_cell_measurement_theta_min      3.3930
_cell_volume                     3801.70(11)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (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 0.985
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_details
;
  1 omega -109.00  -59.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      -36.7513 -178.0000    0.0000 50

  2 omega  -31.00   55.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7513  -38.0000  -30.0000 86

  3 omega  -34.00   65.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7513  -19.0000 -150.0000 99

  4 omega   41.00   76.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000  -45.0000   60.0000 35

  5 omega   40.00  125.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000  -61.0000  -30.0000 85

  6 omega   39.00   77.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000  -45.0000 -150.0000 38

  7 omega   96.00  174.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000   61.0000  120.0000 78

  8 omega   37.00   69.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000  -30.0000 -180.0000 32

  9 omega   37.00   69.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000  -30.0000  150.0000 32

 10 omega   38.00  142.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000  -15.0000  -60.0000 104
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0381799000
_diffrn_orient_matrix_UB_12      0.0756097000
_diffrn_orient_matrix_UB_13      -0.0413159000
_diffrn_orient_matrix_UB_21      0.0389077000
_diffrn_orient_matrix_UB_22      0.0640690000
_diffrn_orient_matrix_UB_23      0.0631987000
_diffrn_orient_matrix_UB_31      0.1023722000
_diffrn_orient_matrix_UB_32      -0.0523116000
_diffrn_orient_matrix_UB_33      0.0176156000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0193
_diffrn_reflns_av_unetI/netI     0.0322
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            11316
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.135
_diffrn_reflns_theta_min         4.449
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.193
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92656
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.388
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.336
_refine_diff_density_min         -0.295
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     512
_refine_ls_number_reflns         7041
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0458
_refine_ls_R_factor_gt           0.0377
_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^)+(0.0579P)^2^+1.0711P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0985
_refine_ls_wR_factor_ref         0.1060
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6034
_reflns_number_total             7041
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce02093g2.cif
_cod_data_source_block           18ssal
_cod_depositor_comments
'Adding full bibliography for 7230048--7230057.cif.'
_cod_original_cell_volume        3801.68(12)
_cod_database_code               7230052
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         Ni4C40H50Cl2O12N12
_reflns_odcompleteness_completeness 98.67
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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:
 C30(H30), C12(H12), C32(H32), C14(H14), C17(H17), C23(H23), C16(H16),
 C15(H15), C19(H19), C1(H1), C33(H33), C35(H35), C34(H34), C20(H20), C5(H5),
 C22(H22), C2(H2), C3(H3), C4(H4), C21(H21)
2.b Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C25(H25A,H25B,H25C), C11(H11A,H11B,H11C), C10(H10A,H10B,
 H10C), C41(H41A,H41B,H41C), C37(H37A,H37B,H37C), C39(H39A,H39B,H39C)
;
_shelx_res_checksum              45680
_olex2_submission_special_instructions 'No special instructions were received'