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_7230048
_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         'C18 H17 N3 O2'
_chemical_formula_sum            'C18 H17 N3 O2'
_chemical_formula_weight         307.34
_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             2016-05-02
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2017-12-04 deposited with the CCDC.
2018-01-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.532(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.4861(3)
_cell_length_b                   7.4773(3)
_cell_length_c                   27.3003(10)
_cell_measurement_reflns_used    2143
_cell_measurement_temperature    173
_cell_measurement_theta_max      71.0850
_cell_measurement_theta_min      5.9720
_cell_volume                     1521.04(10)
_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, 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 0.984
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_details
;
  1 omega   18.00  106.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7513   38.0000 -120.0000 88

  2 omega   44.00   69.00   1.0000    3.1150
omega____ theta____ kappa____ phi______ frames
    -      107.0000  -30.0000  -90.0000 25

  3 omega   41.00  113.00   1.0000    3.1150
omega____ theta____ kappa____ phi______ frames
    -      107.0000  -89.0000 -156.8710 72

  4 omega   47.00   77.00   1.0000    3.1150
omega____ theta____ kappa____ phi______ frames
    -      107.0000  -45.0000 -180.0000 30

  5 omega   90.00  163.00   1.0000    3.1150
omega____ theta____ kappa____ phi______ frames
    -      107.0000   61.0000 -150.0000 73

  6 omega   43.00  129.00   1.0000    3.1150
omega____ theta____ kappa____ phi______ frames
    -      107.0000  -77.0000   90.0000 86

  7 omega   37.00   69.00   1.0000    3.1150
omega____ theta____ kappa____ phi______ frames
    -      107.0000  -30.0000   30.0000 32

  8 omega   37.00   69.00   1.0000    3.1150
omega____ theta____ kappa____ phi______ frames
    -      107.0000  -30.0000   60.0000 32

  9 omega   97.00  175.00   1.0000    3.1150
omega____ theta____ kappa____ phi______ frames
    -      107.0000   45.0000  150.0000 78

 10 omega   19.00  104.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7513   38.0000  150.0000 85

 11 omega -109.00  -78.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -36.7513 -178.0000 -180.0000 31
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0331347000
_diffrn_orient_matrix_UB_12      -0.0035015000
_diffrn_orient_matrix_UB_13      0.0548702000
_diffrn_orient_matrix_UB_21      0.2020022000
_diffrn_orient_matrix_UB_22      -0.0300380000
_diffrn_orient_matrix_UB_23      0.0141544000
_diffrn_orient_matrix_UB_31      0.0292019000
_diffrn_orient_matrix_UB_32      0.2036009000
_diffrn_orient_matrix_UB_33      0.0028910000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0221
_diffrn_reflns_av_unetI/netI     0.0338
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            4473
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.994
_diffrn_reflns_theta_min         6.005
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.725
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88177
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_description       block
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.234
_refine_diff_density_min         -0.182
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         2808
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0482
_refine_ls_R_factor_gt           0.0410
_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^+0.1851P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1040
_refine_ls_wR_factor_ref         0.1111
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2389
_reflns_number_total             2808
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce02093g2.cif
_cod_data_source_block           gekhl
_cod_depositor_comments
'Adding full bibliography for 7230048--7230057.cif.'
_cod_original_cell_volume        1521.04(11)
_cod_database_code               7230048
_shelxl_version_number           2014-1
_chemical_oxdiff_formula         C17H17O3N3
_reflns_odcompleteness_completeness 98.36
_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, All O(H) groups
2.a Me refined with riding coordinates:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C7(H7), C14(H14), C15(H15), C16(H16),
 C17(H17), C18(H18)
2.c Idealised tetrahedral OH refined as rotating group:
 O1(H1)
;
_olex2_submission_special_instructions 'No special instructions were received'