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_7230054
_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
'2(C92 H89 N15 Ni5 O14), 2(Cl O4), 2(Cl0.5 O4), 7(C3 H7 N O)'
_chemical_formula_sum            'C205 H227 Cl3 N37 Ni10 O51'
_chemical_formula_weight         4718.67
_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             2015-11-13
_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                90
_cell_angle_beta                 109.654(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   20.7411(10)
_cell_length_b                   35.8785(14)
_cell_length_c                   18.2934(8)
_cell_measurement_reflns_used    6628
_cell_measurement_temperature    173
_cell_measurement_theta_max      70.8290
_cell_measurement_theta_min      3.7110
_cell_volume                     12820.1(11)
_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, 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 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_details
;
  1 omega   33.00   77.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000 -178.0000    0.0000 44

  2 omega   -7.00  118.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -       54.7500    0.0000 -180.0000 125

  3 omega  -11.00   85.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -       54.7500  -77.0000   30.0000 96

  4 omega   39.00   83.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -50.0000 -180.0000 44

  5 omega   48.00   83.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -50.0000   30.0000 35

  6 omega   37.00   71.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -38.0000 -150.0000 34

  7 omega   40.00   67.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -25.0000   90.0000 27

  8 omega   44.00   83.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -50.0000 -120.0000 39

  9 omega   38.00  148.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -92.0000   30.0000 110

 10 omega   37.00   70.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -38.0000    0.0000 33

 11 omega   38.00   71.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -38.0000  -90.0000 33

 12 omega   99.00  177.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   64.0000  -30.0000 78

 13 omega   40.00   90.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000 -111.0000 -150.0000 50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0730306000
_diffrn_orient_matrix_UB_12      0.0138456000
_diffrn_orient_matrix_UB_13      -0.0448564000
_diffrn_orient_matrix_UB_21      0.0285357000
_diffrn_orient_matrix_UB_22      0.0390721000
_diffrn_orient_matrix_UB_23      -0.0063079000
_diffrn_orient_matrix_UB_31      0.0093316000
_diffrn_orient_matrix_UB_32      -0.0112532000
_diffrn_orient_matrix_UB_33      -0.0769827000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0749
_diffrn_reflns_av_unetI/netI     0.1218
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            43617
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        66.600
_diffrn_reflns_theta_max         66.600
_diffrn_reflns_theta_min         4.634
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.666
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64043
_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            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.222
_exptl_crystal_description       block
_exptl_crystal_F_000             4910
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.339
_refine_diff_density_min         -0.981
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1401
_refine_ls_number_reflns         22143
_refine_ls_number_restraints     62
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.1445
_refine_ls_R_factor_gt           0.0902
_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^)+(0.1265P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2336
_refine_ls_wR_factor_ref         0.2680
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11764
_reflns_number_total             22143
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce02093g2.cif
_cod_data_source_block           azam_ni5
_cod_depositor_comments
'Adding full bibliography for 7230048--7230057.cif.'
_cod_original_cell_volume        12820.1(10)
_cod_database_code               7230054
_chemical_oxdiff_formula         Ni5C100H100N20O30
_reflns_odcompleteness_completeness 98.22
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 O0-Cl1
 1.43 with sigma of 0.02
 Cl1-O044
 1.43 with sigma of 0.02
 Cl1-O040
 1.43 with sigma of 0.02
 O03G-Cl1
 1.43 with sigma of 0.02
3. Rigid bond restraints
 O040, Cl1, O03G, O044, O0
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
O03G \\sim Cl1 \\sim O040 \\sim O044 \\sim O0: within 1.7A with sigma of 0.04
and sigma for terminal atoms of 0.08
5. Rigid body (RIGU) restrains
 O03G, Cl1, O040, O044, O0
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: Cl1(0.5) N3(0.5) O4(0.5) C11(0.5) H11(0.5) C14(0.5) H14A(0.5)
 H14B(0.5) H14C(0.5) C15(0.5) H15A(0.5) H15B(0.5) H15C(0.5)
7.a Rotating group:
 O00S(H00A,H00B)
7.b Ternary CH refined with riding coordinates:
 O1(H1)
7.c Aromatic/amide H refined with riding coordinates:
 C01F(H01F), C01I(H01I), C01L(H01L), C01N(H01N), C01Q(H01Q), C01S(H01S),
 C01U(H01U), C01Z(H01Z), C021(H021), C022(H022), C024(H024), C026(H026),
 C027(H027), C029(H029), C02A(H02D), C02B(H02E), C02C(H02F), C02D(H02G),
 C02E(H02H), C02F(H02I), C02I(H02J), C02J(H02K), C02L(H02L), C02M(H02M),
 C02O(H02Q), C02T(H02X), C02U(H02Y), C02V(H02Z), C02X(H02), C02Y(H0AA),
 C02Z(H1AA), C031(H031), C032(H032), C035(H035), C038(H038), C039(H039),
 C03A(H03A), C03B(H03B), C03D(H03F), C03E(H03G), C03F(H03H), C03H(H03I),
 C03J(H03M), C03L(H3AA), C03N(H03T), C03O(H03U), C03R(H03V), C03S(H03W),
 C03V(H03Z), C03X(H03), C045(H045), C046(H046), C04B(H04J), C11(H11)
7.d Idealised Me refined as rotating group:
 C01H(H01A,H01B,H01C), C01R(H01D,H01E,H01G), C020(H02A,H02B,H02C), C02N(H02N,
 H02O,H02P), C02Q(H02R,H02S,H02T), C02S(H02U,H02V,H02W), C03C(H03C,H03D,H03E),
 C03I(H03J,H03K,H03L), C03K(H03N,H03O,H03P), C03M(H03Q,H03R,H03S), C03T(H03X,
 H03Y,H), C03W(H5AA,HA,HB), C03Y(H2AA,HC,HD), C03Z(H4AA,HE,HF), C042(H04D,H04E,
 H04F), C043(H04G,H04H,H04I), C049(H04A,H04B,H04C), C04C(H04K,H04L,H04M),
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'