Threading of various ‘U’ shaped bidentate axles into a heteroditopic macrocyclic wheel via NiII/ CuII templation
Ghosh, Pradyut; Nandi, Mandira; Santra, Saikat; Akhuli, Bidyut; Dalton Trans.  (2017) –; doi:10.1039/C7DT00699C

data_7042932
_publ_section_title
;
 Threading of various &#x2018;U&#x2019; shaped bidentate axles into a
 heteroditopic macrocyclic wheel via NiII/ CuII templation
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT00699C
_journal_year                    2017
_chemical_formula_moiety
'2(Cl O4), C46 H51 Br2 Cu N7 O8, 2(C H4 O), C2 H3 N'
_chemical_formula_sum            'C50 H62 Br2 Cl2 Cu N8 O18'
_chemical_formula_weight         1357.33
_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
_audit_creation_date             2017-04-28
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2017-05-02 deposited with the CCDC.
2017-05-03 downloaded from the CCDC.
;
_cell_angle_alpha                88.317(2)
_cell_angle_beta                 73.458(2)
_cell_angle_gamma                89.479(2)
_cell_formula_units_Z            2
_cell_length_a                   11.0692(17)
_cell_length_b                   14.524(2)
_cell_length_c                   18.154(3)
_cell_measurement_reflns_used    7398
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      21.845
_cell_measurement_theta_min      2.341
_cell_volume                     2796.6(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.668
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0464
_diffrn_reflns_av_unetI/netI     0.0439
_diffrn_reflns_Laue_measured_fraction_full 0.668
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            25433
_diffrn_reflns_point_group_measured_fraction_full 0.668
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         21.943
_diffrn_reflns_theta_min         1.403
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.995
_exptl_absorpt_correction_T_max  0.7447
_exptl_absorpt_correction_T_min  0.4599
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1549 before and 0.0535 after correction.
The Ratio of minimum to maximum transmission is 0.6176.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.612
_exptl_crystal_description       block
_exptl_crystal_F_000             1390
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.328
_refine_diff_density_min         -1.935
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     766
_refine_ls_number_reflns         6763
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0814
_refine_ls_R_factor_gt           0.0655
_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^)+(0.0823P)^2^+15.9678P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1628
_refine_ls_wR_factor_ref         0.1746
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5484
_reflns_number_total             6763
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00699c2.cif
_cod_data_source_block           MCCU44BR
_cod_original_cell_volume        2796.5(8)
_cod_database_code               7042932
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.943
_shelx_estimated_absorpt_t_min   0.857
_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, All O(H) groups
2. Restrained distances
 N19-C1
 1.13 with sigma of 0.02
3. Rigid bond restraints
 C1, N19
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C1) = Uanis(C0AA)
5. Others
 Sof(Cl2B)=1-FVAR(1)
 Sof(Cl2A)=FVAR(1)
 Fixed Sof: O16(0.42435) O15(0.47632) O14(0.39663) O16A(0.57565) O15A(0.52368)
 O14A(0.60337)
6.a Ternary CH refined with riding coordinates:
 N3(H3), N5(H5), N4(H4)
6.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C17(H17A,H17B), C8(H8A,H8B), C29(H29A,H29B), C3AA(H3AA,H3AB),
 C22(H22A,H22B), C7(H7A,H7B), C20(H20A,H20B), C18(H18A,H18B), C21(H21A,H21B),
 C46(H46A,H46B), C42(H42A,H42B), C45(H45A,H45B), C43(H43A,H43B)
6.c Aromatic/amide H refined with riding coordinates:
 C16(H16), C25(H25), C15(H15), C12(H12), C28(H28), C13(H13), C24(H24),
 C1AA(H1AA), C26(H26), C6(H6), C2AA(H2AA), C2(H2), N2(H2A), N1(H1), C32(H32),
 C34(H34), C39(H39), C37(H37), C40(H40), C31(H31)
6.d Idealised Me refined as rotating group:
 C48(H48A,H48B,H48C), C47(H47A,H47B,H47C), C0AA(H0AA,H0AB,H0AC)
6.e Idealised tetrahedral OH refined as rotating group:
 O18(H18), O17(H17)
;
_shelx_res_checksum              94101
_olex2_submission_special_instructions 'No special instructions were received'