Polynuclear alkoxy-zinc complexes of bowl-shaped macrocycles and their use in the copolymerisation of cyclohexene oxide and CO<sub>2</sub>.
Pankhurst, James R.; Paul, Shyeni; Zhu, Yunqing; Williams, Charlotte K.; Love, Jason B.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 4887–4893; doi:10.1039/c9dt00595a

data_7049389
_publ_section_title
;
 Polynuclear alkoxy-zinc complexes of bowl-shaped macrocycles and their
 use in the copolymerisation of cyclohexene oxide and CO<sub>2</sub>.
;
_journal_issue                   15
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4887
_journal_page_last               4893
_journal_paper_doi               10.1039/c9dt00595a
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C59 H52 F10 N8 O3 Zn3, 3.5(C6 H6)'
_chemical_formula_sum            'C80 H73 F10 N8 O3 Zn3'
_chemical_formula_weight         1580.57
_chemical_properties_physical    ', Moisture-sensitive'
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2016-10-06
_audit_creation_method
;
Olex2 1.2
(compiled Feb 16 2016 13:09:46 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-10-11 deposited with the CCDC.    2019-03-12 downloaded from the CCDC.
;
_cell_angle_alpha                105.877(2)
_cell_angle_beta                 105.185(2)
_cell_angle_gamma                104.788(2)
_cell_formula_units_Z            2
_cell_length_a                   13.6817(3)
_cell_length_b                   17.1958(4)
_cell_length_c                   17.9104(4)
_cell_measurement_reflns_used    16653
_cell_measurement_temperature    170
_cell_measurement_theta_max      27.7320
_cell_measurement_theta_min      3.2410
_cell_volume                     3660.91(17)
_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
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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, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      170
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1042
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -25.00   23.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      -19.2955  -99.0000   30.0000 48

  2 omega  -25.00   23.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      -19.2955  -99.0000  150.0000 48

  3 omega  -25.00   64.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       22.1080  -99.0000    0.0000 89

  4 omega  -47.00   43.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       22.1080  -57.0000  120.0000 90

  5 omega  -47.00   43.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       22.1080  -57.0000 -120.0000 90

  6 omega    1.00   91.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       22.1080   57.0000   30.0000 90

  7 omega    1.00   91.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       22.1080   57.0000  150.0000 90

  8 omega   34.00   98.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       22.1080  179.0000  150.0000 64

  9 omega  -25.00   64.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       22.1080  -99.0000 -180.0000 89

 10 omega  -47.00   43.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       22.1080  -57.0000    0.0000 90

 11 omega    1.00   91.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       22.1080   57.0000  -90.0000 90

 12 omega  -25.00   23.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      -19.2955  -99.0000  -90.0000 48

 13 omega  -89.00   11.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      -19.2955  -77.0000  120.0000 100

 14 omega  -25.00   64.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       22.1080  -99.0000   60.0000 89

 15 omega   -3.00   95.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       22.1080   38.0000  -60.0000 98

 16 omega  -25.00   64.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       22.1080  -99.0000  -60.0000 89

 17 omega   34.00   66.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       22.1080  179.0000  -30.0000 32
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0151920000
_diffrn_orient_matrix_UB_12      -0.0316623000
_diffrn_orient_matrix_UB_13      0.0172558000
_diffrn_orient_matrix_UB_21      0.0429672000
_diffrn_orient_matrix_UB_22      0.0264962000
_diffrn_orient_matrix_UB_23      0.0381882000
_diffrn_orient_matrix_UB_31      -0.0348891000
_diffrn_orient_matrix_UB_32      0.0198723000
_diffrn_orient_matrix_UB_33      0.0136513000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0631
_diffrn_reflns_av_unetI/netI     0.0445
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            88885
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.681
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_min         2.964
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.055
_exptl_absorpt_correction_T_max  0.780
_exptl_absorpt_correction_T_min  0.472
_exptl_absorpt_correction_type   analytical
_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)
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)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_description       block
_exptl_crystal_F_000             1626
_exptl_crystal_recrystallization_method
'Slow diffusion of hexane into a benzene solution'
_exptl_crystal_size_max          0.4378
_exptl_crystal_size_mid          0.4149
_exptl_crystal_size_min          0.1279
_refine_diff_density_max         0.547
_refine_diff_density_min         -0.391
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     946
_refine_ls_number_reflns         13872
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0579
_refine_ls_R_factor_gt           0.0401
_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^)+(0.0280P)^2^+3.4810P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0816
_refine_ls_wR_factor_ref         0.0880
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10986
_reflns_number_total             13872
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00595a2.cif
_cod_data_source_block           j15064c
_cod_depositor_comments          'Adding full bibliography for 7049389.cif.'
_cod_original_cell_volume        3660.90(17)
_cod_database_code               7049389
_chemical_oxdiff_formula         'C50 H30 F10 N8 Zn4 O4'
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.63
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 C63, C64, C65, C60, C61, C62
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(H54A)=Sof(C56B)=Sof(H56D)=Sof(H56E)=Sof(H56F)=1-FVAR(1)
 Sof(H54)=Sof(C56A)=Sof(H56A)=Sof(H56B)=Sof(H56C)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C6(H6), C31(H31), C51(H51), C54(H54A), C54(H54), C57(H57)
4.b Aromatic/amide H refined with riding coordinates:
 N7(H7), 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), C72(H72), C73(H73), C74(H74), C75(H75), C76(H76), C77(H77),
 C66(H66), C67(H67), C68(H68), C69(H69), C70(H70), C71(H71), C63(H63), C64(H64),
  C65(H65), C60(H60), C61(H61), C62(H62), C02C(H02C), C02O(H02O), C02Q(H02Q)
4.c Fitted hexagon refined as free rotating group:
 C63(C64,C65,C60,C61,C62)
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), C53(H53A,H53B,H53C), C55(H55A,H55B,H55C),
 C56A(H56A,H56B,H56C), C56B(H56D,H56E,H56F), C58(H58A,H58B,H58C), C59(H59A,H59B,
 H59C)
;
_shelx_res_checksum              68958
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'