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_7230056
_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         'C76 H78 N12 Ni4 O12, 2(Cl O4), 5(C2 H6 O)'
_chemical_formula_sum            'C86 H108 Cl2 N12 Ni4 O25'
_chemical_formula_weight         2015.58
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2015-12-01
_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                90
_cell_angle_beta                 107.926(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.2703(7)
_cell_length_b                   28.8077(12)
_cell_length_c                   22.7473(9)
_cell_measurement_reflns_used    12426
_cell_measurement_temperature    173
_cell_measurement_theta_max      69.6330
_cell_measurement_theta_min      4.2700
_cell_volume                     9520.8(7)
_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 0.980
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_details
;
  1 omega  -22.00   24.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000   90.0000 46

  2 omega  -67.00  -24.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000   90.0000 43

  3 omega  -94.00  -18.00   1.0000   32.5000
omega____ theta____ kappa____ phi______ frames
    -      -54.7500  125.0000 -180.0000 76

  4 omega   23.00  128.00   1.0000   32.5000
omega____ theta____ kappa____ phi______ frames
    -       54.7500   38.0000 -150.0000 105

  5 omega   61.00   87.00   1.0000   32.5000
omega____ theta____ kappa____ phi______ frames
    -       54.7500  -77.0000  -60.0000 26

  6 omega  -12.00   57.00   1.0000   32.5000
omega____ theta____ kappa____ phi______ frames
    -       54.7500  -77.0000  -60.0000 69

  7 omega   37.00  149.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -92.0000   30.0000 112

  8 omega   35.00   71.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -25.0000 -180.0000 36

  9 omega   43.00   83.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -50.0000    0.0000 40

 10 omega  125.00  151.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -92.0000  -30.0000 26

 11 omega   37.00  107.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -92.0000  -30.0000 70

 12 omega   41.00   67.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -25.0000 -150.0000 26

 13 omega   76.00  177.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   77.0000  120.0000 101

 14 omega   84.00  149.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   50.0000 -150.0000 65

 15 omega  110.00  151.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   38.0000    0.0000 41
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0881619000
_diffrn_orient_matrix_UB_12      0.0295475000
_diffrn_orient_matrix_UB_13      0.0138437000
_diffrn_orient_matrix_UB_21      -0.0582145000
_diffrn_orient_matrix_UB_22      0.0446243000
_diffrn_orient_matrix_UB_23      -0.0082923000
_diffrn_orient_matrix_UB_31      0.0088987000
_diffrn_orient_matrix_UB_32      -0.0005947000
_diffrn_orient_matrix_UB_33      0.0692683000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0335
_diffrn_reflns_av_unetI/netI     0.0513
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.949
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            32761
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.949
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.099
_diffrn_reflns_theta_min         4.429
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.059
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80529
_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    1.406
_exptl_crystal_description       block
_exptl_crystal_F_000             4216
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.293
_refine_diff_density_min         -0.883
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1174
_refine_ls_number_reflns         17467
_refine_ls_number_restraints     145
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0941
_refine_ls_R_factor_gt           0.0754
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1494P)^2^+3.8390P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2190
_refine_ls_wR_factor_ref         0.2432
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13110
_reflns_number_total             17467
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce02093g2.cif
_cod_data_source_block           5ssal
_cod_depositor_comments
'Adding full bibliography for 7230048--7230057.cif.'
_cod_original_cell_volume        9520.9(7)
_cod_database_code               7230056
_chemical_oxdiff_formula         Ni4C120H120N30O50Cl4
_reflns_odcompleteness_completeness 98.17
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.46
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H00C of O00C, H00A of O00A, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, H009 of O009, H00L of O00L, H9 of O9, H01I of O01H, H4
  of O4, H5 of O5, H7 of O7
2. Restrained distances
 O009-H009
 0.85 with sigma of 0.01
 O00L-H00L
 0.85 with sigma of 0.01
 C6-C4
 1.53 with sigma of 0.02
 C5-C13
 1.53 with sigma of 0.02
 C9-C8
 1.53 with sigma of 0.02
 C1-C3
 1.53 with sigma of 0.02
 C02J-C035
 1.53 with sigma of 0.02
 C2-C7
 1.53 with sigma of 0.02
 C2-O5
 1.43 with sigma of 0.02
 O9-C8
 1.43 with sigma of 0.02
 O4-C6
 1.43 with sigma of 0.02
 O5-C2
 1.43 with sigma of 0.02
 C1-O7
 1.43 with sigma of 0.02
 C8-O9
 1.43 with sigma of 0.02
 C9-C8
 1.53 with sigma of 0.02
 C2-C7
 1.53 with sigma of 0.02
 C1-C3
 1.53 with sigma of 0.02
 C02J-H009
 1.86007 with sigma of 0.02
 Ni03-H009
 2.691536 with sigma of 0.02
 C5-H00L
 1.848625 with sigma of 0.02
 Ni04-H00L
 2.617007 with sigma of 0.02
3. Rigid bond restraints
 C2, O5, C7, C1, O7, C3, O9, C8, C9, O4, H4, C6, C4, H6A, H6B, H4A, H4B, H4C
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C13, C5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(O7) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C8) \\sim
Ueq, Uanis(O9) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(O4)
\\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(O5) \\sim Ueq,
Uanis(C2) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
5. Rigid body (RIGU) restrains
 C2, O5, C7, O7, C1, C3, C4, O4, H4, C6, H6A, H6B, H4A, H4B, H4C, O9, C8, C9
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C5, C13
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Riding coordinates:
 O00A(H00A), O7(H7)
6.b Ternary CH refined with riding coordinates:
 O00C(H00C)
6.c Secondary CH2 refined with riding coordinates:
 C02J(H02E,H02J), C5(H5A,H5B), C1(H1A,H1B), C2(H2A,H2B), C6(H6A,H6B),
 C02U(H2AA,HF), C8(H8A,H8B)
6.d Me refined with riding coordinates:
 C02O(H02N,H02O,H02P), C02P(H02Q,H02R,H02S), C02R(H02U,H02V,H02W), C02W(H02Y,H,
 HA), C13(H13A,H13B,H13C), C020(H0AA,HB,HC), C028(H1AA,HD,HE), C035(H03A,H03B,
 H03C), C3(H3A,H3B,H3C), C7(H7A,H7B,H7C), C4(H4A,H4B,H4C), C033(H03D,H03E,H03F),
  C9(H9A,H9B,H9C)
6.e Aromatic/amide H refined with riding coordinates:
 C00S(H00S), C00U(H00U), C00X(H00X), C01C(H01C), C01G(H01G), C01J(H01J),
 C01L(H01L), C01O(H01O), C01R(H01R), C01S(H01S), C01T(H01T), C01U(H01U),
 C01V(H01V), C01X(H01X), C01Y(H01Y), C01Z(H01Z), C02A(H02A), C02B(H02B),
 C02C(H02C), C02D(H02D), C02F(H02F), C02G(H02G), C02H(H02H), C02I(H02I),
 C02K(H02K), C02L(H02L), C02M(H02M), C02Q(H02T), C02V(H02X), C02X(H02Z),
 C02Z(H02), C014(H014), C015(H015), C016(H016), C019(H019), C022(H022),
 C023(H023), C026(H026), C027(H027), C031(H031)
6.f Idealised Me refined as rotating group:
 C01W(H01A,H01B,H01D), C010(H01E,H01F,H01H)
6.g Idealised tetrahedral OH refined as rotating group:
 O5(H5), O4(H4), O01H(H01I), O9(H9)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'