Isoskeletal Schiff base polynuclear coordination clusters: synthetic and theoretical aspects
Griffiths, Kieran; Dokorou, Vassiliki N.; Spencer, John; Abdul-Sada, Alaa; Vargas, Alfredo; Kostakis, George E.; CrystEngComm 18 (2016) 704–; doi:10.1039/C5CE02109J

data_7223507
_publ_section_title
;
 Isoskeletal Schiff base polynuclear coordination clusters: synthetic and
 theoretical aspects
;
_journal_issue                   5
_journal_name_full               CrystEngComm
_journal_page_first              704
_journal_paper_doi               10.1039/C5CE02109J
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         'C76 H68 N4 Ni4 O16, 6(C H4 O)'
_chemical_formula_sum            'C82 H92 N4 Ni4 O22'
_chemical_formula_weight         1716.36
_chemical_name_systematic
;
 ?
;
_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     iterative
_audit_creation_date             2015-01-13
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.12 svn.r3133 for OlexSys, GUI svn.r4987)
;
_audit_update_record
;
2015-11-15 deposited with the CCDC.
2015-12-17 downloaded from the CCDC.
;
_cell_angle_alpha                71.347(2)
_cell_angle_beta                 71.670(2)
_cell_angle_gamma                67.774(2)
_cell_formula_units_Z            4
_cell_length_a                   18.0377(13)
_cell_length_b                   18.3422(13)
_cell_length_c                   29.900(2)
_cell_measurement_temperature    100
_cell_volume                     8462.6(10)
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.967
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0854
_diffrn_reflns_av_unetI/netI     0.0739
_diffrn_reflns_laue_measured_fraction_full 0.977
_diffrn_reflns_laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            106354
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        27.500
_diffrn_reflns_theta_max         27.613
_diffrn_reflns_theta_min         2.245
_exptl_absorpt_coefficient_mu    0.941
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.653
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm
;
_exptl_crystal_colour            'dark yellow'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.262
_exptl_crystal_description       prism
_exptl_crystal_F_000             3348
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.910
_refine_diff_density_min         -1.152
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1922
_refine_ls_number_reflns         38045
_refine_ls_number_restraints     206
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0845
_refine_ls_R_factor_gt           0.0643
_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^)+(0.1110P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1750
_refine_ls_wR_factor_ref         0.1896
_reflns_Friedel_coverage         0.000
_reflns_number_gt                27858
_reflns_number_total             38045
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce02109j3.cif
_cod_data_source_block           14_CCDC_1406230
_cod_depositor_comments
'Adding full bibliography for 7223506--7223525.cif.'
_cod_original_cell_volume        8462.6(11)
_cod_database_code               7223507
_shelxl_version_number           2014-1
_olex2_refinement_description
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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. Restrained distances
 O25-H25A
 0.85 with sigma of 0.01
 O55-H55
 0.85 with sigma of 0.01
 O68-H68
 0.85 with sigma of 0.01
 O70-H70
 0.85 with sigma of 0.01
 O77-H77
 0.85 with sigma of 0.01
 O92-H92
 0.85 with sigma of 0.01
 O98-H98A
 0.85 with sigma of 0.01
 O101-H101
 0.85 with sigma of 0.01
 C22-O1
 1.43 with sigma of 0.02
 O6-C28
 1.43 with sigma of 0.02
 O3-C31
 1.43 with sigma of 0.02
 C10-O12
 1.43 with sigma of 0.02
 O2-C7
 1.43 with sigma of 0.02
 C141-H25A
 1.88654 with sigma of 0.02
 Ni2-H25A
 2.64075 with sigma of 0.02
 C1D-H55
 1.869418 with sigma of 0.02
 Ni12-H55
 2.654961 with sigma of 0.02
 C213-H68
 1.864016 with sigma of 0.02
 Ni15-H68
 2.638839 with sigma of 0.02
 C152-H70
 1.887571 with sigma of 0.02
 Ni13-H70
 2.628461 with sigma of 0.02
 C207-H77
 1.896255 with sigma of 0.02
 Ni4-H77
 2.670523 with sigma of 0.02
 C197-H92
 1.876459 with sigma of 0.02
 Ni10-H92
 2.64467 with sigma of 0.02
 C29-H98A
 1.900785 with sigma of 0.02
 Ni5-H98A
 2.656038 with sigma of 0.02
 C56-H101
 1.859479 with sigma of 0.02
 Ni8-H101
 2.659212 with sigma of 0.02
3. Rigid bond restraints
 C7, H7A, H7B, H7C, O2, H2A, C31, H31A, H31B, O3, H3A, C22, H22A, H22B, H22C,
 O1, H1, C28, H28A, H28B, H28C, O6, H6A, C10, H10D, H10E, H10F, O12, H12
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C7 \\sim H7A \\sim H7B \\sim H7C \\sim O2 \\sim H2A \\sim C31 \\sim H31A \\sim
H31B \\sim H31C \\sim O3 \\sim H3A \\sim C22 \\sim H22B \\sim H22C \\sim O1
\\sim H1 \\sim C28 \\sim H28A \\sim H28B \\sim H28C \\sim O6 \\sim H6A \\sim
C10 \\sim H10D \\sim H10E \\sim H10F \\sim O12 \\sim H12: within 1.7A with
sigma of 0.04 and sigma for terminal atoms of 0.08
5. Rigid body (RIGU) restrains
 C7, H7A, H7B, H7C, O2, H2A, C31, H31A, H31B, H31C, O3, H3A, C22, H22A, H22B,
 H22C, O1, H1, C28, H28A, H28B, H28C, O6, H6A, C10, H10D, H10E, H10F, O12, H12
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Me refined with riding coordinates:
 C11(H11A,H11B,H11C), C29(H29A,H29B,H29C), C56(H56A,H56B,H56C), C79(H79A,H79B,
 H79C), C124(H12A,H12B,H12C), C152(H15A,H15B,H15C), C165(H16A,H16B,H16C),
 C213(H21A,H21B,H21C), C1(H1B,H1D,H1E), C1D(H1DA,H1DB,H1DC), C1G(H1GA,H1GB,
 H1GC), C118(H11D,H11E,H11F), C141(H14A,H14B,H14C), C197(H19A,H19B,H19C),
 C207(H20A,H20B,H20C), C31(H31A,H31B,H31C), C22(H22A,H22B,H22C), C28(H28A,H28B,
 H28C), C10(H10D,H10E,H10F)
6.b Aromatic/amide H refined with riding coordinates:
 C1A(H1A), C1C(H1C), C1F(H1F), C1H(H1H), C1K(H1K), C2(H2), C3(H3), C4AA(H4AA),
 C6(H6), C8(H8), C9(H9), C16(H16), C20(H20), C24(H24), C26(H26), C27(H27),
 C35(H35), C36(H36), C48(H48), C53(H53), C76(H76), C87(H87), C91(H91), C94(H94),
  C98(H98), C108(H108), C110(H110), C114(H114), C117(H117), C122(H122),
 C132(H132), C139(H139), C148(H148), C164(H164), C169(H169), C184(H184),
 C188(H188), C219(H219), C232(H232), C238(H238), C0AA(H0AA), C1B(H1BA),
 C1E(H1EA), C1I(H1I), C1J(H1J), C15(H15), C18(H18), C19(H19), C23(H23),
 C25(H25), C33(H33), C38(H38), C39(H39), C42(H42), C43(H43), C44(H44), C47(H47),
  C49(H49), C52(H52), C59(H59), C63(H63), C69(H69), C73(H73), C81(H81),
 C82(H82), C99(H99), C107(H107), C115(H115), C119(H119), C121(H121), C134(H134),
  C137(H137), C145(H145), C167(H167), C171(H171), C181(H181), C185(H185),
 C196(H196), C240(H240), C241(H241)
6.c Idealised Me refined as rotating group:
 C104(H10A,H10B,H10C), C7(H7A,H7B,H7C)
6.d Idealised tetrahedral OH refined as rotating group:
 O2(H2A), O3(H3A), O1(H1), O6(H6A), O12(H12)
;
_olex2_submission_special_instructions 'No special instructions were received'