Macrocyclic Platforms for the Construction of Tetranuclear Oxo and Hydroxo Zinc Clusters
Cadenbach, Thomas; Pankhurst, James R.; Hofmann, Tommy A.; Curcio, Massimiliano; Arnold, Polly L.; Love, Jason B.; Organometallics 34 (2015) 2608–; doi:10.1021/om501244n

data_4085518
_publ_section_title
;
 Macrocyclic Platforms for the Construction of Tetranuclear Oxo and
 Hydroxo Zinc Clusters
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              2608
_journal_paper_doi               10.1021/om501244n
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C62 H56 F10 N8 O3 Zn4'
_chemical_formula_sum            'C62 H40 F10 N8 O3 Zn4'
_chemical_formula_weight         1396.50
_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             2014-12-03
_audit_creation_method
;
Olex2 1.2
(compiled 2014.11.28 svn.r3107 for OlexSys, GUI svn.r4957)
;
_cell_angle_alpha                90
_cell_angle_beta                 94.577(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.5879(5)
_cell_length_b                   19.5250(6)
_cell_length_c                   20.8445(7)
_cell_measurement_reflns_used    16897
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.3640
_cell_measurement_theta_min      3.3450
_cell_volume                     6729.6(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 8.0521
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0480
_diffrn_reflns_av_unetI/netI     0.0554
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            55629
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.024
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.483
_exptl_absorpt_correction_T_max  0.951
_exptl_absorpt_correction_T_min  0.573
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.378
_exptl_crystal_description       block
_exptl_crystal_F_000             2808
_exptl_crystal_size_max          0.8173
_exptl_crystal_size_mid          0.4652
_exptl_crystal_size_min          0.0622
_refine_diff_density_max         0.599
_refine_diff_density_min         -0.540
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     812
_refine_ls_number_reflns         13739
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0830
_refine_ls_R_factor_gt           0.0480
_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^)+(0.0684P)^2^+6.5743P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1230
_refine_ls_wR_factor_ref         0.1403
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9459
_reflns_number_total             13739
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om501244n_si_002.cif
_cod_data_source_block           J14006_Zn4O_compound_3
_cod_depositor_comments
'Adding full bibliography for 4085516--4085519.cif.'
_cod_database_code               4085518
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C54-C53 \\sim C54A-C53
 with sigma of 0.02
 C52-C51 \\sim C52A-C51
 with sigma of 0.02
3. Others
 Sof(H53C)=Sof(H53D)=Sof(C54A)=Sof(H54D)=Sof(H54E)=Sof(H54F)=1-FVAR(1)
 Sof(H53A)=Sof(H53B)=Sof(C54)=Sof(H54A)=Sof(H54B)=Sof(H54C)=FVAR(1)
 Sof(H51C)=Sof(H51D)=Sof(C52A)=Sof(H52D)=Sof(H52E)=Sof(H52F)=1-FVAR(2)
 Sof(H51A)=Sof(H51B)=Sof(C52)=Sof(H52A)=Sof(H52B)=Sof(H52C)=FVAR(2)
4.a Ternary CH refined with riding coordinates:
 C0AA(H0AA), C31(H31)
4.b Secondary CH2 refined with riding coordinates:
 C51(H51A,H51B), C51(H51C,H51D), C53(H53A,H53B), C53(H53C,H53D), C55(H55A,
 H55B), C56(H56A,H56B), C57(H57A,H57B), C58(H58A,H58B), C59(H59A,H59B),
 C60(H60A,H60B), C61(H61A,H61B), C62(H62A,H62B)
4.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C4(H4), C14(H14), C15(H15), C17(H17), C19(H19), C22(H22),
 C26(H26), C28(H28), C29(H29), C39(H39), C40(H40), C42(H42), C44(H44), C47(H47)
4.d Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C49(H49A,H49B,H49C), C50(H50A,H50B,
 H50C), C52(H52A,H52B,H52C), C54(H54A,H54B,H54C), C54A(H54D,H54E,H54F),
 C52A(H52D,H52E,H52F)
;
_shelx_res_checksum              13155
_shelx_hkl_checksum              43258
_shelx_fab_checksum              63405
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'