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_4125722
_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         'C228 H258 N24 O12 Zn6, 6(C4 N), 9(O)'
_chemical_formula_sum            'C252 H258 N30 O21 Zn6'
_chemical_formula_weight         4435.09
_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                   43.652(2)
_cell_length_b                   43.652(2)
_cell_length_c                   11.4512(7)
_cell_measurement_reflns_used    8844
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      55
_cell_measurement_theta_min      4.05
_cell_volume                     18896.9(17)
_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 0.974
_diffrn_measured_fraction_theta_max 0.974
_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  0.1203
_diffrn_reflns_av_unetI/netI     0.1409
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            24339
_diffrn_reflns_point_group_measured_fraction_full 0.840
_diffrn_reflns_point_group_measured_fraction_max 0.840
_diffrn_reflns_theta_full        54.996
_diffrn_reflns_theta_max         54.996
_diffrn_reflns_theta_min         4.051
_exptl_absorpt_coefficient_mu    1.145
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.169
_exptl_crystal_description       block
_exptl_crystal_F_000             6984
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.726
_refine_diff_density_min         -0.478
_refine_diff_density_rms         0.072
_refine_ls_abs_structure_details
;
 Flack x determined using 1542 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.12(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     754
_refine_ls_number_reflns         8844
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.1348
_refine_ls_R_factor_gt           0.0886
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1109P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2048
_refine_ls_wR_factor_ref         0.2299
_reflns_Friedel_coverage         0.725
_reflns_Friedel_fraction_full    0.706
_reflns_Friedel_fraction_max     0.706
_reflns_number_gt                5843
_reflns_number_total             8844
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            R-1_2-butylamine.cif
_cod_data_source_block           CIF-3
_cod_depositor_comments
;

2021-08-29
Space group name changed to comply with IUCR recomendations
                 miguel
;
_cod_original_cell_volume        18897(2)
_cod_database_code               4125722
_shelx_estimated_absorpt_t_max   0.894
_shelx_estimated_absorpt_t_min   0.875
_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
 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
 1.53 with sigma of 0.02
 C78-C79
 1.55 with sigma of 0.02
 C79-C80
 1.53 with sigma of 0.02
 C77-C79
 2.38 with sigma of 0.02
 C77-N9
 2.38 with sigma of 0.02
 C79-N9
 2.38 with sigma of 0.02
 C78-C80
 2.38 with sigma of 0.02
 C80-N9
 3.3 with sigma of 0.02
 N9-C78
 1.48 with sigma of 0.02
 C81-C82
 1.53 with sigma of 0.02
 C82-C83
 1.55 with sigma of 0.02
 C83-C84
 1.53 with sigma of 0.02
 N10-C82
 1.5 with sigma of 0.02
 C82-C84
 2.65 with sigma of 0.02
 C81-N10
 2.45 with sigma of 0.02
 N10-C83
 2.45 with sigma of 0.02
 C81-C83
 2.4 with sigma of 0.02
 C84-N10
 3 with sigma of 0.02
 O5-O6
 2.95 with sigma of 0.02
 N10-O6
 3.05 with sigma of 0.02
 N10-O7
 3.05 with sigma of 0.02
 N9-O5
 2.95 with sigma of 0.02
 N9-O6
 3.05 with sigma of 0.02
3.a Fixed occupancy and ADP/Uiso:
 C77, C78, N9, C79, C80, C81, C82, N10, C83, C84, O6, O5, O7
3.b Ternary CH refined with riding coordinates:
 C17(H17), C22(H22), C55(H55), C60(H60)
3.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)
3.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)
3.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)
3.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'