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_4085517
_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_absolute_configuration ad
_chemical_formula_moiety         'C86 H82 F10 N8 O4 Zn4'
_chemical_formula_sum            'C86 H82 F10 N8 O4 Zn4'
_chemical_formula_weight         1743.07
_space_group_crystal_system      trigonal
_space_group_IT_number           161
_space_group_name_Hall           'R 3 -2"c'
_space_group_name_H-M_alt        'R 3 c :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2014-10-07
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   24.4911(4)
_cell_length_b                   24.4911(4)
_cell_length_c                   89.0912(17)
_cell_measurement_reflns_used    16106
_cell_measurement_temperature    170.0
_cell_measurement_theta_max      24.5680
_cell_measurement_theta_min      3.3340
_cell_volume                     46278.8(14)
_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      170.0
_diffrn_detector_area_resol_mean 16.1042
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega  -96.00   60.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.3078   19.0000   60.0000 156

  2 omega  -25.00   29.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.3078  -99.0000    0.0000 54

  3 omega  -29.00   48.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       21.6359  -77.0000  -60.0000 77

  4 omega  -15.00   74.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       21.6359   77.0000  -90.0000 89
;
_diffrn_measurement_device_type  'Agilent Technologies XCalibur'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0251816000
_diffrn_orient_matrix_UB_12      0.0218011000
_diffrn_orient_matrix_UB_13      -0.0045788000
_diffrn_orient_matrix_UB_21      -0.0188424000
_diffrn_orient_matrix_UB_22      0.0126900000
_diffrn_orient_matrix_UB_23      -0.0025254000
_diffrn_orient_matrix_UB_31      0.0112968000
_diffrn_orient_matrix_UB_32      0.0219617000
_diffrn_orient_matrix_UB_33      0.0060061000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0438
_diffrn_reflns_av_unetI/netI     0.0376
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       91
_diffrn_reflns_limit_l_min       -108
_diffrn_reflns_number            92030
_diffrn_reflns_point_group_measured_fraction_full 0.950
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        23.249
_diffrn_reflns_theta_max         23.249
_diffrn_reflns_theta_min         3.003
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.983
_exptl_absorpt_correction_T_max  0.410
_exptl_absorpt_correction_T_min  0.299
_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            'dark yellow'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.126
_exptl_crystal_description       block
_exptl_crystal_F_000             16128
_exptl_crystal_size_max          0.9868
_exptl_crystal_size_mid          0.7507
_exptl_crystal_size_min          0.6993
_refine_diff_density_max         0.517
_refine_diff_density_min         -0.426
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details
;
 Flack x determined using 5248 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.003(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1324
_refine_ls_number_reflns         14042
_refine_ls_number_restraints     1111
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0516
_refine_ls_R_factor_gt           0.0435
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0924P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1202
_refine_ls_wR_factor_ref         0.1267
_reflns_Friedel_coverage         0.905
_reflns_Friedel_fraction_full    0.903
_reflns_Friedel_fraction_max     0.903
_reflns_number_gt                12365
_reflns_number_total             14042
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om501244n_si_002.cif
_cod_data_source_block           j14030_Zn4Et4_compound_2b
_cod_depositor_comments
'Adding full bibliography for 4085516--4085519.cif.'
_cod_original_cell_volume        46278.9(17)
_cod_database_code               4085517
_chemical_oxdiff_formula         'Zn4 C60 H60 O4 F10 N8'
_reflns_odcompleteness_completeness 99.69
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_olex2_refinement_description
;
1. Shared sites
{F1A, F1B}
{O4A, O4B}
{C66B, C66A}
{H26A, H26}
{H69C, H70C}
2. Others
 Fixed Uiso: H62A(0.134) H62B(0.134) H61A(0.183) H61B(0.183) H60A(0.137)
 H60B(0.137) H59A(0.109) H59B(0.109) H71A(0.094) H71B(0.094) H72A(0.132)
 H72B(0.132) H73A(0.161) H73B(0.161) H74A(0.14) H74B(0.14) H71C(0.141)
 H71D(0.141) H72C(0.175) H72D(0.175) H73C(0.172) H73D(0.172) H74C(0.144)
 H74D(0.144) H80A(0.128) H80B(0.128) H79A(0.31) H79B(0.31) H78A(0.235)
 H78B(0.235) H77A(0.162) H77B(0.162) H80C(0.109) H80D(0.109) H79C(0.163)
 H79D(0.163) H78C(0.099) H78D(0.099) H77C(0.077) H77D(0.077) H65A(0.077)
 H65B(0.077) H66A(0.207) H66B(0.207) H67A(0.149) H67B(0.149) H68A(0.081)
 H68B(0.081) H65C(0.125) H65D(0.125) H66C(0.185) H66D(0.185) H67C(0.166)
 H67D(0.166) H68C(0.128) H68D(0.128) H1A(0.044) H1B(0.053) H3(0.066) H4(0.069)
 H6(0.06) H8(0.085) H9(0.09) H10(0.077) H12(0.065) H14(0.074) H15(0.083)
 H16(0.073) H19(0.058) H21(0.06) H23(0.083) H24(0.086) H26(0.071) H26A(0.071)
 H34(0.088) H35(0.077) H37(0.06) H39(0.07) H40(0.074) H41(0.072) H43(0.059)
 H45(0.074) H46(0.08) H47(0.078) H50(0.054) H52(0.06) H54(0.061) H55(0.057)
 H57A(0.143) H57B(0.143) H58A(0.302) H58B(0.302) H58C(0.302) H63A(0.121)
 H63B(0.121) H64A(0.216) H64B(0.216) H64C(0.216) H69A(0.13) H69B(0.13)
 H69C(0.154) H69D(0.154) H70A(0.312) H70B(0.312) H70C(0.312) H70D(0.366)
 H70E(0.366) H70F(0.366) H75A(0.105) H75B(0.105) H75C(0.136) H75D(0.136)
 H76A(0.261) H76B(0.261) H76C(0.261) H76D(0.18) H76E(0.18) H76F(0.18)
 Fixed X: H62A(0.8082) H62B(0.8793) H61A(0.8385) H61B(0.9001) H60A(0.9561)
 H60B(0.9065) H59A(0.9211) H59B(0.8662) H71A(0.7231) H71B(0.6594) H72A(0.6265)
 H72B(0.6936) H73A(0.6425) H73B(0.5988) H74A(0.6646) H74B(0.7162) H71C(0.7063)
 H71D(0.6678) H72C(0.6258) H72D(0.6014) H73C(0.6384) H73D(0.687) H74C(0.7056)
 H74D(0.7575) H80A(1.1668) H80B(1.1569) H79A(1.1301) H79B(1.1429) H78A(1.0412)
 H78B(1.0305) H77A(0.9889) H77B(1.0209) H80C(1.1384) H80D(1.1634) H79C(1.1393)
 H79D(1.1225) H78C(1.0254) H78D(1.0391) H77C(0.9963) H77D(0.9881) H65A(1.1061)
 H65B(1.047) H66A(1.092) H66B(1.0219) H67A(0.994) H67B(1.0587) H68A(0.9484)
 H68B(1.0003) H65C(1.0209) H65D(1.0913) H66C(1.0842) H66D(1.0312) H67C(0.9515)
 H67D(1.0016) H68C(1.0281) H68D(0.9574) H1A(0.9007) H1B(0.8981) H3(0.7597)
 H4(0.6627) H6(0.6451) H8(0.6716) H9(0.6068) H10(0.5728) H12(0.5741) H14(0.576)
 H15(0.612) H16(0.675) H19(0.7094) H21(0.684) H23(0.7509) H24(0.8466)
 H26(0.9377) H26A(0.9372) H34(0.8429) H35(0.9185) H37(1.0525) H39(1.175)
 H40(1.2713) H41(1.3121) H43(1.3054) H45(1.3013) H46(1.2523) H47(1.1518)
 H50(1.1105) H52(1.0435) H54(0.9136) H55(0.8331) H57A(0.9081) H57B(0.8792)
 H58A(0.8539) H58B(0.8491) H58C(0.7925) H63A(1.0749) H63B(1.079) H64A(1.1774)
 H64B(1.1732) H64C(1.177) H69A(0.8744) H69B(0.8328) H69C(0.7965) H69D(0.8662)
 H70A(0.8309) H70B(0.7615) H70C(0.8033) H70D(0.849) H70E(0.8578) H70F(0.7888)
 H75A(1.0792) H75B(1.1465) H75C(1.1515) H75D(1.0977) H76A(1.1524) H76B(1.1697)
 H76C(1.1019) H76D(1.1908) H76E(1.1406) H76F(1.1946)
 Fixed Y: H62A(0.0469) H62B(0.0825) H61A(0.089) H61B(0.0855) H60A(0.1872)
 H60B(0.1901) H59A(0.2229) H59B(0.2178) H71A(0.242) H71B(0.1756) H72A(0.2198)
 H72B(0.2537) H73A(0.1693) H73B(0.1258) H74A(0.0901) H74B(0.146) H71C(0.2112)
 H71D(0.1483) H72C(0.1674) H72D(0.0984) H73C(0.083) H73D(0.157) H74C(0.0695)
 H74D(0.1337) H80A(0.4672) H80B(0.4064) H79A(0.4136) H79B(0.362) H78A(0.3026)
 H78B(0.3301) H77A(0.3504) H77B(0.4064) H80C(0.4675) H80D(0.4555) H79C(0.3793)
 H79D(0.3526) H78C(0.2982) H78D(0.3535) H77C(0.3401) H77D(0.3792) H65A(0.5191)
 H65B(0.4596) H66A(0.5744) H66B(0.5184) H67A(0.5794) H67B(0.6136) H68A(0.5021)
 H68B(0.5521) H65C(0.4592) H65D(0.5072) H66C(0.5897) H66D(0.542) H67C(0.5259)
 H67D(0.5978) H68C(0.5706) H68D(0.5118) H1A(0.2995) H1B(0.2977) H3(0.3223)
 H4(0.217) H6(0.0936) H8(-0.0017) H9(-0.1113) H10(-0.1609) H12(-0.1559) H14(-
 0.1536) H15(-0.0973) H16(0.0134) H19(0.0621) H21(0.1147) H23(0.2416)
 H24(0.3362) H26(0.3111) H26A(0.3128) H34(0.3964) H35(0.5124) H37(0.5822)
 H39(0.6059) H40(0.7016) H41(0.744) H43(0.737) H45(0.7317) H46(0.6789)
 H47(0.5881) H50(0.551) H52(0.565) H54(0.4853) H55(0.3769) H57A(0.1391)
 H57B(0.1572) H58A(0.0618) H58B(0.0373) H58C(0.0437) H63A(0.3966) H63B(0.3726)
 H64A(0.4212) H64B(0.4817) H64C(0.4682) H69A(0.1395) H69B(0.075) H69C(0.1001)
 H69D(0.1518) H70A(0.0569) H70B(0.0381) H70C(0.1028) H70D(0.0492) H70E(0.0848)
 H70F(0.0336) H75A(0.3915) H75B(0.4509) H75C(0.4126) H75D(0.3655) H76A(0.3628)
 H76B(0.3912) H76C(0.3314) H76D(0.4216) H76E(0.4391) H76F(0.4864)
 Fixed Z: H62A(-0.0197) H62B(-0.0133) H61A(-0.0424) H61B(-0.0377) H60A(-
 0.0335) H60B(-0.0449) H59A(-0.0161) H59B(-0.0269) H71A(-0.0713) H71B(-0.0688)
 H72A(-0.086) H72B(-0.0945) H73A(-0.1093) H73B(-0.0958) H74A(-0.094) H74B(-
 0.1044) H71C(-0.0829) H71D(-0.073) H72C(-0.0981) H72D(-0.0912) H73C(-0.1124)
 H73D(-0.1147) H74C(-0.0992) H74D(-0.1072) H80A(-0.0327) H80B(-0.0419) H79A(-
 0.0121) H79B(-0.02) H78A(-0.0276) H78B(-0.0121) H77A(-0.0362) H77B(-0.024)
 H80C(-0.0182) H80D(-0.0338) H79C(-0.0124) H79D(-0.0293) H78C(-0.0191) H78D(-
 0.0073) H77C(-0.0365) H77D(-0.023) H65A(0.0439) H65B(0.0517) H66A(0.0606)
 H66B(0.0644) H67A(0.0521) H67B(0.0427) H68A(0.0359) H68B(0.0245) H65C(0.0544)
 H65D(0.0488) H66C(0.0543) H66D(0.0658) H67C(0.0505) H67D(0.0461) H68C(0.025)
 H68D(0.0263) H1A(-0.0004) H1B(0.0106) H3(0.0062) H4(0.0043) H6(0.0027)
 H8(0.0255) H9(0.0242) H10(0.002) H12(-0.026) H14(-0.0535) H15(-0.0754) H16(-
 0.075) H19(-0.0237) H21(-0.037) H23(-0.0265) H24(-0.0366) H26(-0.0594) H26A(-
 0.0584) H34(-0.0621) H35(-0.0583) H37(-0.0556) H39(-0.0779) H40(-0.076) H41(-
 0.0534) H43(-0.0256) H45(0.0021) H46(0.0233) H47(0.0226) H50(-0.0287) H52(-
 0.0138) H54(-0.0225) H55(-0.014) H57A(0.0163) H57B(0.0302) H58A(0.0372)
 H58B(0.0204) H58C(0.0274) H63A(0.0323) H63B(0.016) H64A(0.0252) H64B(0.0303)
 H64C(0.0128) H69A(-0.083) H69B(-0.0742) H69C(-0.0952) H69D(-0.0896) H70A(-
 0.0992) H70B(-0.0936) H70C(-0.1025) H70D(-0.0854) H70E(-0.0698) H70F(-0.0754)
 H75A(-0.0857) H75B(-0.0824) H75C(-0.0592) H75D(-0.0704) H76A(-0.0837) H76B(-
 0.0671) H76C(-0.0704) H76D(-0.0828) H76E(-0.0893) H76F(-0.078)
;
_shelx_res_checksum              92143
_shelx_hkl_checksum              19001
_shelx_fab_checksum              50426
_shelx_shelxl_version_number     2014/7
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems Desktop Cooler'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a glass fibre in perfluoroether oil'
_olex2_submission_special_instructions 'No special instructions were received'