Chiral NH-Controlled Supramolecular Metallacycles.
Dong, Jinqiao; Tan, Chunxia; Zhang, Kang; Liu, Yan; Low, Paul J.; Jiang, Jianwen; Cui, Yong; Journal of the American Chemical Society 139 (2017) 1554–1564; doi:10.1021/jacs.6b11422

data_4125724
_publ_section_title
;
 Chiral NH-Controlled Supramolecular Metallacycles.
;
_journal_issue                   4
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1554
_journal_page_last               1564
_journal_paper_doi               10.1021/jacs.6b11422
_journal_volume                  139
_journal_year                    2017
_chemical_absolute_configuration rmad
_chemical_formula_moiety         '6(C4 O), C228 H258 N24 O12 Zn6, 6(O)'
_chemical_formula_sum            'C252 H258 N24 O24 Zn6'
_chemical_formula_weight         4399.03
_space_group_crystal_system      trigonal
_space_group_IT_number           146
_space_group_name_Hall           'R 3'
_space_group_name_H-M_alt        'R 3 :H'
_symmetry_space_group_name_Hall  'R 3'
_symmetry_space_group_name_H-M   'R 3 :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-10-09
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   43.6574(17)
_cell_length_b                   43.6574(17)
_cell_length_c                   11.5213(6)
_cell_measurement_reflns_used    6553
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      50
_cell_measurement_theta_min      4.49
_cell_volume                     19017.3(14)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1246
_diffrn_reflns_av_unetI/netI     0.1909
_diffrn_reflns_Laue_measured_fraction_full 0.965
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            14989
_diffrn_reflns_point_group_measured_fraction_full 0.754
_diffrn_reflns_point_group_measured_fraction_max 0.754
_diffrn_reflns_theta_full        49.979
_diffrn_reflns_theta_max         49.979
_diffrn_reflns_theta_min         4.494
_exptl_absorpt_coefficient_mu    1.136
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.152
_exptl_crystal_description       block
_exptl_crystal_F_000             6930
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.876
_refine_diff_density_min         -0.563
_refine_diff_density_rms         0.101
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.09(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     752
_refine_ls_number_reflns         6553
_refine_ls_number_restraints     357
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.1260
_refine_ls_R_factor_gt           0.0959
_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^)+(0.1166P)^2^+10.2819P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2256
_refine_ls_wR_factor_ref         0.2520
_reflns_Friedel_coverage         0.561
_reflns_Friedel_fraction_full    0.542
_reflns_Friedel_fraction_max     0.542
_reflns_number_gt                4897
_reflns_number_total             6553
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            R-1_2-butanol.cif
_cod_data_source_block           CIF-4
_cod_depositor_comments
;

2021-08-29
Space group name changed to comply with IUCR recomendations
                 miguel
;
_cod_original_cell_volume        19017.2(18)
_cod_database_code               4125724
_shelx_estimated_absorpt_t_max   0.905
_shelx_estimated_absorpt_t_min   0.885
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C3-C6
 1.55 with sigma of 0.02
 C12-C14
 1.54 with sigma of 0.02
 C12-C10
 1.53 with sigma of 0.02
 C12-C15
 1.54 with sigma of 0.02
 C28-C30
 1.5 with sigma of 0.02
 C30-C31
 1.5 with sigma of 0.02
 C50-C51
 1.5 with sigma of 0.02
 C50-C53
 1.5 with sigma of 0.02
 C48-C50
 1.5 with sigma of 0.02
 C68-C71
 1.52 with sigma of 0.02
 C64-C68
 1.5 with sigma of 0.02
 C20-C21
 1.5 with sigma of 0.02
 C55-C56
 1.52 with sigma of 0.02
 C77-C78
 1.5 with sigma of 0.02
 O5-C78
 1.478 with sigma of 0.02
 C78-C79
 1.52 with sigma of 0.02
 C79-C80
 1.52 with sigma of 0.02
 C80-C78
 2.35 with sigma of 0.02
 C77-C79
 2.35 with sigma of 0.02
 C77-O5
 2.35 with sigma of 0.02
 O5-C79
 2.37 with sigma of 0.02
 O6-C82
 1.53 with sigma of 0.02
 C81-C82
 1.515 with sigma of 0.02
 C82-C83
 1.575 with sigma of 0.02
 C82-C84
 2.6 with sigma of 0.02
 C83-C84
 1.485 with sigma of 0.02
 C81-C84
 2.8 with sigma of 0.02
 C81-C83
 2.36 with sigma of 0.02
 C81-O6
 2.36 with sigma of 0.02
 O6-C83
 2.36 with sigma of 0.02
 O5-O7
 3.16 with sigma of 0.02
 O6-O8
 3.15 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(N3) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C5) \\sim
Ueq, Uanis(C12) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C13) \\sim Ueq,
Uanis(C15) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C22)
\\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C38) \\sim Ueq,
Uanis(C44) \\sim Ueq, Uanis(C57) \\sim Ueq, Uanis(C65) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C38) \\sim Ueq, Uanis(N5) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C43)
\\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C47) \\sim Ueq, Uanis(C49) \\sim Ueq,
Uanis(C52) \\sim Ueq, Uanis(C56) \\sim Ueq, Uanis(C58) \\sim Ueq, Uanis(C59)
\\sim Ueq, Uanis(C69) \\sim Ueq, Uanis(C71) \\sim Ueq, Uanis(C73) \\sim Ueq,
Uanis(C75) \\sim Ueq, Uanis(C76) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C70) \\sim Ueq, Uanis(C74) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(N2) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(C3) \\sim
Ueq, Uanis(C7) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C11)
\\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C25) \\sim Ueq,
Uanis(C26) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C40)
\\sim Ueq, Uanis(C41) \\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(C48) \\sim Ueq,
Uanis(C66) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C28) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4.a Fixed occupancy and ADP/Uiso:
 C83, O6, C81, C82, O5, C77, C78, C79, C80, O7, O8
4.b Ternary CH refined with riding coordinates:
 C17(H17), C22(H22), C55(H55), C60(H60)
4.c Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,
 H21B), C56(H56A,H56B), C57(H57A,H57B), C58(H58A,H58B), C59(H59A,H59B),
 C61(H61A,H61B)
4.d Me refined with riding coordinates:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C32(H32A,H32B,
 H32C), C31(H31A,H31B,H31C), C33(H33A,H33B,H33C), C51(H51A,H51B,H51C), C52(H52A,
 H52B,H52C), C53(H53A,H53B,H53C), C69(H69A,H69B,H69C), C70(H70A,H70B,H70C),
 C71(H71A,H71B,H71C)
4.e Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C7(H7), C11(H11), C25(H25), C27(H27),
 C35(H35), C36(H36), C37(H37), C38(H38), C39(H39), C40(H40), C42(H42), C43(H43),
  C45(H45), C49(H49), C54(H54), C65(H65), C67(H67), C23(H23), C73(H73),
 C74(H74), C75(H75), C76(H76)
4.f Fitted hexagon refined as free rotating group:
 N1(C1,C2,C3,C4,C5), C6(C7,C8,C9,C10,C11), C24(C25,C26,C27,C28,C29), C34(C35,
 C36,N4,C37,C38), N5(C39,C40,C41,C42,C43), C44(C45,C46,C47,C48,C49), C62(C63,
 C64,C65,C66,C67), C72(C73,C74,N8,C75,C76)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'