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_4085519
_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 H28 F9.98 N8 O4 Zn4, C4 H8 O'
_chemical_formula_sum            'C66 H36 F9.98 N8 O5 Zn4'
_chemical_formula_weight         1472.13
_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   geom
_audit_creation_date             2014-12-02
_audit_creation_method
;
Olex2 1.2
(compiled 2014.11.28 svn.r3107 for OlexSys, GUI svn.r4957)
;
_cell_angle_alpha                104.772(4)
_cell_angle_beta                 99.895(3)
_cell_angle_gamma                102.885(4)
_cell_formula_units_Z            2
_cell_length_a                   12.5794(3)
_cell_length_b                   14.5209(8)
_cell_length_c                   21.8649(10)
_cell_measurement_reflns_used    20894
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.1170
_cell_measurement_theta_min      3.3750
_cell_volume                     3652.2(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_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    'SIR-92 (Altomare, 1994)'
_diffrn_ambient_temperature      173.15
_diffrn_detector_area_resol_mean 8.0521
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.922
_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  0.0945
_diffrn_reflns_av_unetI/netI     0.0788
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.922
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            83941
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.922
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.224
_diffrn_reflns_theta_min         3.023
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.372
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.41817
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_description       block
_exptl_crystal_F_000             1476
_exptl_crystal_size_max          0.3120
_exptl_crystal_size_mid          0.2660
_exptl_crystal_size_min          0.1000
_refine_diff_density_max         5.395
_refine_diff_density_min         -0.975
_refine_diff_density_rms         0.205
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     938
_refine_ls_number_reflns         18282
_refine_ls_number_restraints     267
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.1379
_refine_ls_R_factor_gt           0.0992
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2673
_refine_ls_wR_factor_ref         0.3069
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11480
_reflns_number_total             18282
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om501244n_si_002.cif
_cod_data_source_block           j14034_Zn4(OH)4_compound_4
_cod_depositor_comments
'Adding full bibliography for 4085516--4085519.cif.'
_cod_database_code               4085519
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(F1B) = Uanis(F1A) = Uanis(F2A) = Uanis(F3A) = Uanis(F4A) = Uanis(F5A) =
Uanis(F5B) = Uanis(F4B) = Uanis(F3B) = Uanis(F2B)
3. Rigid body (RIGU) restrains
 F1A, F1B, F2A, F2B, F3A, F3B, F4A, F4B, F5A, F5B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F6A, F6B, F7A, F7B, F8A, F8B, F9A, F9B, F10A, F10B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C52A, C52B, C53A, C53B, C54A, C54B, C55A, C55B, C56A, C56B, C57A, C57B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C58A, C58B, C59A, C59B, C60A, C60B, C61A, C61B, C62A, C62B, C63A, C63B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(C52B)=Sof(C53B)=Sof(C54B)=Sof(C55B)=Sof(C56B)=Sof(C57B)=1-FVAR(1)
 Sof(C52A)=Sof(C53A)=Sof(C54A)=Sof(C55A)=Sof(C56A)=Sof(C57A)=FVAR(1)
 Sof(C58B)=Sof(C59B)=Sof(C60B)=Sof(C61B)=Sof(C62B)=Sof(C63B)=1-FVAR(2)
 Sof(C58A)=Sof(C59A)=Sof(C60A)=Sof(C61A)=Sof(C62A)=Sof(C63A)=FVAR(2)
 Sof(F1B)=Sof(F2B)=Sof(F3B)=Sof(F4B)=Sof(F5B)=1-FVAR(3)
 Sof(F1A)=Sof(F2A)=Sof(F3A)=Sof(F4A)=Sof(F5A)=FVAR(3)
 Sof(F6B)=Sof(F7B)=Sof(F9B)=Sof(F10B)=1-FVAR(4)
 Sof(F6A)=Sof(F7A)=Sof(F8A)=Sof(F9A)=Sof(F10A)=Sof(F8B)=FVAR(4)
5.a Secondary CH2 refined with riding coordinates:
 C64(H64A,H64B), C65(H65A,H65B), C66(H66A,H66B), C67(H67A,H67B)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C8(H8), C9(H9), C10(H10), C12(H12), C14(H14),
 C15(H15), C16(H16), C19(H19), C22(H22), C24(H24), C25(H25), C29(H29), C30(H30),
  C32(H32), C34(H34), C35(H35), C36(H36), C38(H38), C40(H40), C41(H41),
 C42(H42), C45(H45), C47(H47), C49(H49), C50(H50)
5.c Fitted hexagon refined as free rotating group:
 C52A(C53A,C54A,C55A,C56A,C57A), C58A(C59A,C60A,C61A,C62A,C63A), C52B(C53B,
 C54B,C55B,C56B,C57B), C58B(C59B,C60B,C61B,C62B,C63B)
;
_shelx_res_checksum              33648
_shelx_hkl_checksum              80479
_shelx_fab_checksum              13778
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'