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_7230055
_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
'C82 H82 N12 Ni4 O12, 2(Cl O4), H2 O, 2(C2 H3 N)'
_chemical_formula_sum            'C86 H90 Cl2 N14 Ni4 O21'
_chemical_formula_weight         1961.45
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2015-11-13
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_audit_update_record
;
2017-12-04 deposited with the CCDC.
2018-01-29 downloaded from the CCDC.
;
_cell_angle_alpha                87.743(3)
_cell_angle_beta                 85.594(2)
_cell_angle_gamma                79.606(3)
_cell_formula_units_Z            2
_cell_length_a                   14.8923(4)
_cell_length_b                   17.0968(7)
_cell_length_c                   17.3958(6)
_cell_measurement_reflns_used    10158
_cell_measurement_temperature    173
_cell_measurement_theta_max      71.0670
_cell_measurement_theta_min      4.2520
_cell_volume                     4342.1(3)
_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, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2008)'
_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 0.935
_diffrn_measurement_details
;
  1 omega  -31.00   51.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.3763  -57.0000  -60.0000 82

  2 omega    9.00   66.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.3763  -19.0000    0.0000 57

  3 omega    1.00   75.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.3763  -99.0000  -90.0000 74

  4 omega   80.00  134.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000  -93.0000   -2.2913 54

  5 omega   89.00  115.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000  -93.0000   60.3315 26

  6 omega   80.00  107.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000  -93.0000  126.5741 27

  7 omega   47.00   73.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000  -93.0000   -2.2913 26

  8 omega   42.00   67.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000  -45.0000  -30.0000 25

  9 omega   43.00   69.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000  -30.0000  -30.0000 26

 10 omega   38.00   63.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000  -30.0000  -60.0000 25

 11 omega   46.00   76.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000  -45.0000  -90.0000 30

 12 omega   48.00   74.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000  -45.0000 -120.0000 26

 13 omega   97.00  124.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000  -91.0000 -116.9276 27

 14 omega   77.00  169.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000   15.0000  -90.0000 92

 15 omega   76.00  171.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000   15.0000    0.0000 95

 16 omega   59.00  100.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.3763   77.0000 -180.0000 41

 17 omega   25.00  102.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.3763   38.0000 -180.0000 77

 18 omega   39.00   67.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000  -30.0000 -150.0000 28

 19 omega   41.00   67.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000  -30.0000 -180.0000 26

 20 omega   45.00   74.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000  -91.0000 -116.9276 29

 21 omega   46.00  126.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000  -92.0000  -76.0000 80

 22 omega   40.00   66.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000  -30.0000   30.0000 26

 23 omega   38.00   66.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000  -30.0000    0.0000 28

 24 omega   43.00   68.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000  -45.0000   30.0000 25

 25 omega   37.00   68.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000  -30.0000   90.0000 31

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

 27 omega   38.00   63.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000  -30.0000  120.0000 25

 28 omega   43.00   77.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000  -45.0000  150.0000 34

 29 omega   43.00   70.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000  -93.0000  126.5741 27

 30 omega   44.00  120.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000  -93.0000  166.3509 76
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0309233000
_diffrn_orient_matrix_UB_12      -0.0402494000
_diffrn_orient_matrix_UB_13      0.0766946000
_diffrn_orient_matrix_UB_21      -0.0156439000
_diffrn_orient_matrix_UB_22      -0.0804668000
_diffrn_orient_matrix_UB_23      -0.0281701000
_diffrn_orient_matrix_UB_31      0.0995800000
_diffrn_orient_matrix_UB_32      -0.0174187000
_diffrn_orient_matrix_UB_33      -0.0349149000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0489
_diffrn_reflns_av_unetI/netI     0.0634
_diffrn_reflns_Laue_measured_fraction_full 0.955
_diffrn_reflns_Laue_measured_fraction_max 0.935
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            27717
_diffrn_reflns_point_group_measured_fraction_full 0.955
_diffrn_reflns_point_group_measured_fraction_max 0.935
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.257
_diffrn_reflns_theta_min         4.603
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.216
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72299
_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            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.500
_exptl_crystal_description       block
_exptl_crystal_F_000             2036
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.682
_refine_diff_density_min         -0.778
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1163
_refine_ls_number_reflns         15772
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0639
_refine_ls_R_factor_gt           0.0529
_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^)+(0.0680P)^2^+1.1620P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1308
_refine_ls_wR_factor_ref         0.1419
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13025
_reflns_number_total             15772
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce02093g2.cif
_cod_data_source_block           ss18a
_cod_depositor_comments
'Adding full bibliography for 7230048--7230057.cif.'
_cod_database_code               7230055
_chemical_oxdiff_formula         Ni4C80H90O20N10Cl2
_reflns_odcompleteness_completeness 95.66
_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,H) groups
2.a Free rotating group:
 O00W(H00A,H00B)
2.b Aromatic/amide H refined with riding coordinates:
 C010(H010), C011(H011), C01D(H01D), C01E(H01E), C01F(H01F), C01J(H01J),
 C01P(H01P), C01Q(H01Q), C01R(H01R), C01S(H01S), C01T(H01T), C01U(H01U),
 C01X(H01X), C01Y(H01Y), C01Z(H01Z), C020(H020), C024(H024), C025(H025),
 C028(H028), C02A(H02D), C02C(H02E), C02D(H02F), C02E(H02G), C02F(H02H),
 C02G(H02I), C02H(H02J), C02I(H02K), C02J(H02L), C02K(H02M), C02L(H02N),
 C02N(H02O), C02O(H02P), C02Q(H02T), C02S(H02X), C02T(H02Y), C02U(H02Z),
 C030(H030), C031(H031), C035(H035), C036(H036)
2.c Idealised Me refined as rotating group:
 C01I(H01A,H01B,H01C), C021(H02A,H02B,H02C), C02P(H02Q,H02R,H02S), C02R(H02U,
 H02V,H02W), C02V(H02,H,HA), C02W(H0AA,HB,HC), C02X(H1AA,HD,HE), C033(H03A,H03B,
 H03C), C034(H03D,H03E,H03F), C037(H03G,H03H,H03I), C038(H03J,H03K,H03L),
 C039(H03M,H03N,H03O), C03B(H03V,H03W,H03X), C03F(H03Y,HF,HG), C03G(H03P,H03Q,
 H03R), C03H(H03S,H03T,H03U)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'