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_4085516
_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
'C35 H46 F10 N8 O2 Zn2'
_chemical_formula_sum            'C35 H46 F10 N8 O2 Zn2'
_chemical_formula_weight         1351.38
_chemical_name_systematic
;
 ?
;
_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   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 114.868(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.2526(7)
_cell_length_b                   32.0839(14)
_cell_length_c                   31.1888(15)
_cell_measurement_reflns_used    13211
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      23.5990
_cell_measurement_theta_min      3.2460
_cell_volume                     14755.4(12)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_molecular_graphics    ortep
_computing_publication_material  ortep
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, SHELXL-2014)'
_computing_structure_solution    SIR-92
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.853
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1276
_diffrn_reflns_av_unetI/netI     0.2140
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.853
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            101227
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.853
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.384
_diffrn_reflns_theta_min         2.959
_exptl_absorpt_coefficient_mu    0.721
_exptl_absorpt_correction_T_max  0.938
_exptl_absorpt_correction_T_min  0.870
_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    1.217
_exptl_crystal_description       plate
_exptl_crystal_F_000             5500
_exptl_crystal_size_max          0.6411
_exptl_crystal_size_mid          0.1615
_exptl_crystal_size_min          0.0893
_refine_diff_density_max         1.153
_refine_diff_density_min         -0.943
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.963
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1633
_refine_ls_number_reflns         28568
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.963
_refine_ls_R_factor_all          0.2083
_refine_ls_R_factor_gt           0.1055
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1478P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2624
_refine_ls_wR_factor_ref         0.3154
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11790
_reflns_number_total             28568
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om501244n_si_002.cif
_cod_data_source_block           j14036_Zn2_compound_1b
_cod_depositor_comments
'Adding full bibliography for 4085516--4085519.cif.'
_cod_original_cell_volume        14755.3(12)
_cod_database_code               4085516
_shelxl_version_number           2014-3
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H1(0.082) H3(0.078) H4(0.069) H6(0.053) H8(0.058) H9(0.054)
 H10(0.059) H12(0.046) H14(0.054) H15(0.055) H16(0.053) H19(0.046) H21(0.055)
 H23(0.059) H24(0.063) H26(0.058) H28(0.064) H29(0.06) H31(0.045) H33(0.056)
 H34(0.051) H35(0.055) H37(0.051) H39(0.07) H40(0.073) H41(0.067) H44(0.041)
 H46(0.067) H48(0.099) H49(0.097) H63A(0.104) H63B(0.104) H64A(0.153)
 H64B(0.153) H65A(0.148) H65B(0.148) H66A(0.123) H66B(0.123) H67A(0.091)
 H67B(0.091) H68A(0.168) H68B(0.168) H69A(0.126) H69B(0.126) H70A(0.088)
 H70B(0.088) H71(0.063) H73(0.079) H74(0.077) H76(0.053) H78(0.057) H79(0.062)
 H80(0.056) H82(0.046) H84(0.058) H85(0.06) H86(0.059) H89(0.046) H91(0.056)
 H93(0.076) H94(0.072) H96(0.061) H98(0.085) H99(0.085) H101(0.062) H103(0.069)
 H104(0.077) H105(0.07) H107(0.05) H109(0.047) H110(0.047) H111(0.053)
 H114(0.044) H116(0.048) H118(0.057) H119(0.071) H13A(0.09) H13B(0.09)
 H13C(0.115) H13D(0.115) H13E(0.137) H13F(0.137) H13G(0.088) H13H(0.088)
 H13I(0.129) H13J(0.129) H138(0.165) H13K(0.112) H13L(0.112) H14A(0.092)
 H14B(0.092)
 Fixed X: H1(0.3383) H3(0.1547) H4(0.0496) H6(0.0908) H8(0.2959) H9(0.2946)
 H10(0.22) H12(0.1179) H14(0.0201) H15(-0.0548) H16(-0.0522) H19(0.1231) H21(-
 0.0976) H23(-0.1534) H24(-0.058) H26(0.1353) H28(0.3182) H29(0.4243)
 H31(0.3928) H33(0.2015) H34(0.226) H35(0.3287) H37(0.4248) H39(0.5242)
 H40(0.58) H41(0.5568) H44(0.3708) H46(0.5824) H48(0.6236) H49(0.52)
 H63A(0.2634) H63B(0.2306) H64A(0.2878) H64B(0.3181) H65A(0.4587) H65B(0.423)
 H66A(0.4745) H66B(0.4746) H67A(0.2243) H67B(0.2649) H68A(0.2228) H68B(0.2026)
 H69A(0.0574) H69B(0.0767) H70A(0.0335) H70B(0.0058) H71(0.6191) H73(0.4735)
 H74(0.3737) H76(0.3949) H78(0.4183) H79(0.388) H80(0.4495) H82(0.5471)
 H84(0.6493) H85(0.7478) H86(0.774) H89(0.6037) H91(0.5824) H93(0.554)
 H94(0.6699) H96(0.8582) H98(1.0385) H99(1.1296) H101(1.0714) H103(1.031)
 H104(1.0313) H105(0.9408) H107(0.8319) H109(0.7313) H110(0.6532) H111(0.6632)
 H114(0.8509) H116(0.8766) H118(0.9289) H119(0.8282) H13A(0.5081) H13B(0.4751)
 H13C(0.5257) H13D(0.5043) H13E(0.6453) H13F(0.6634) H13G(0.7329) H13H(0.7001)
 H13I(0.7521) H13J(0.8414) H138(0.8333) H13K(0.9861) H13L(0.9143) H14A(0.9197)
 H14B(0.9798)
 Fixed Y: H1(0.2968) H3(0.2551) H4(0.3117) H6(0.4001) H8(0.4797) H9(0.5492)
 H10(0.5669) H12(0.5477) H14(0.5289) H15(0.4798) H16(0.41) H19(0.4081)
 H21(0.3662) H23(0.2809) H24(0.217) H26(0.2163) H28(0.2132) H29(0.2729)
 H31(0.3566) H33(0.4079) H34(0.4738) H35(0.5183) H37(0.5355) H39(0.5555)
 H40(0.5387) H41(0.4724) H44(0.405) H46(0.3936) H48(0.3046) H49(0.2528)
 H63A(0.3974) H63B(0.441) H64A(0.4405) H64B(0.4783) H65A(0.4533) H65B(0.4058)
 H66A(0.4502) H66B(0.4005) H67A(0.3412) H67B(0.3182) H68A(0.26) H68B(0.2822)
 H69A(0.2694) H69B(0.2546) H70A(0.3355) H70B(0.3141) H71(0.1229) H73(0.1067)
 H74(0.1689) H76(0.2565) H78(0.3084) H79(0.3801) H80(0.4268) H82(0.4405)
 H84(0.4566) H85(0.4337) H86(0.363) H89(0.2987) H91(0.2805) H93(0.1889)
 H94(0.1329) H96(0.1657) H98(0.1435) H99(0.2055) H101(0.2941) H103(0.3665)
 H104(0.4365) H105(0.4595) H107(0.4431) H109(0.4296) H110(0.3827) H111(0.3102)
 H114(0.301) H116(0.2588) H118(0.1696) H119(0.1068) H13A(0.2467) H13B(0.2255)
 H13C(0.1614) H13D(0.1792) H13E(0.1831) H13F(0.1554) H13G(0.2096) H13H(0.2391)
 H13I(0.2714) H13J(0.2434) H138(0.2808) H13K(0.308) H13L(0.3457) H14A(0.3496)
 H14B(0.3079)
 Fixed Z: H1(0.2665) H3(0.1695) H4(0.1166) H6(0.107) H8(0.1838) H9(0.16)
 H10(0.0812) H12(-0.0003) H14(-0.083) H15(-0.1389) H16(-0.1173) H19(0.0446)
 H21(-0.0529) H23(-0.0402) H24(-0.0129) H26(-0.0309) H28(0.08) H29(0.0954)
 H31(0.0529) H33(-0.0692) H34(-0.0916) H35(-0.0391) H37(0.0444) H39(0.1281)
 H40(0.2075) H41(0.2319) H44(0.0943) H46(0.2037) H48(0.2393) H49(0.2506)
 H63A(0.2676) H63B(0.2401) H64A(0.3278) H64B(0.3035) H65A(0.3532) H65B(0.3482)
 H66A(0.2854) H66B(0.2921) H67A(-0.1202) H67B(-0.0698) H68A(-0.1009) H68B(-
 0.1506) H69A(-0.1716) H69B(-0.1189) H70A(-0.1573) H70B(-0.1185) H71(-0.0353)
 H73(0.023) H74(0.0153) H76(-0.0118) H78(-0.0875) H79(-0.1014) H80(-0.0418)
 H82(0.0441) H84(0.1272) H85(0.2002) H86(0.2168) H89(0.0703) H91(0.1357)
 H93(0.135) H94(0.1743) H96(0.2702) H98(0.249) H99(0.2424) H101(0.2204)
 H103(0.2526) H104(0.2324) H105(0.1577) H107(0.0755) H109(-0.0056) H110(-
 0.0651) H111(-0.0497) H114(0.1127) H116(0.0595) H118(0.083) H119(0.0616) H13A(-
 0.1437) H13B(-0.1067) H13C(-0.1151) H13D(-0.1669) H13E(-0.1517) H13F(-0.1056)
 H13G(-0.0625) H13H(-0.1084) H13I(0.291) H13J(0.305) H138(0.3733) H13K(0.3774)
 H13L(0.3643) H14A(0.295) H14B(0.3055)
;
_shelx_res_checksum              9743
_shelx_hkl_checksum              96416
_shelx_fab_checksum              34804