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_7042930
_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(C42 H49 Cu N7 O4), 4(Cl O4), 2(C1.50 H3 N0.50)'
_chemical_formula_sum            'C87 H104 Cl4 Cu2 N15 O24'
_chemical_formula_weight         2012.75
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-04-04
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2017-04-13 deposited with the CCDC.
2017-05-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.300(3)
_cell_length_b                   18.907(4)
_cell_length_c                   19.051(4)
_cell_measurement_reflns_used    6251
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      18.09
_cell_measurement_theta_min      2.15
_cell_volume                     4790.6(18)
_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 0.495
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0542
_diffrn_reflns_av_unetI/netI     0.0475
_diffrn_reflns_Laue_measured_fraction_full 0.495
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            19974
_diffrn_reflns_point_group_measured_fraction_full 0.482
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         19.537
_diffrn_reflns_theta_min         1.517
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.635
_exptl_absorpt_correction_T_max  0.981
_exptl_absorpt_correction_T_min  0.955
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2004/1 (Bruker,2004) was used for absorption correction.
R(int) was 0.0827 before and 0.0586 after correction.
The Ratio of minimum to maximum transmission is 0.7544.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.395
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2098
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.436
_refine_diff_density_min         -0.223
_refine_diff_density_rms         0.047
_refine_ls_abs_structure_details
;
 Flack x determined using 1494 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.025(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     592
_refine_ls_number_reflns         4170
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0556
_refine_ls_R_factor_gt           0.0490
_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^)+(0.0450P)^2^+7.8986P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1178
_refine_ls_wR_factor_ref         0.1215
_reflns_Friedel_coverage         0.757
_reflns_Friedel_fraction_full    0.466
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                3749
_reflns_number_total             4170
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00699c2.cif
_cod_data_source_block           MCCU44BP
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'MULTI-SCAN' changed to
'multi-scan' according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_cell_volume        4790.7(17)
_cod_database_code               7042930
_shelxl_version_number           2014/6
_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. Others
 Fixed Sof: C2(0.5) N10(0.5)
3.a Ternary CH refined with riding coordinates:
 N5(HI), N4(HJ), N3(HK)
3.b Secondary CH2 refined with riding coordinates:
 C18(HO,HP), C4AA(HU,HV), C33(H0AA,H1AA), C34(H2AA,H3AA), C36(H4AA,H5AA),
 C38(H6AA,H7AA), C40(H0BA,H1BA), C39(H2BA,H3BA), C44(H8BA,H9BA), C43(H0CA,H1CA)
3.c Aromatic/amide H refined with riding coordinates:
 C5AA(H), C6AA(HA), C5(HB), C11(HC), C1(HD), C3AA(HE), C2AA(HL), C0AA(HM),
 C1AA(HN), C24(HQ), C25(HR), C22(HS), C21(HT), C45(HW), C27(HX), C29(HY),
 C31(HZ), N6(H8AA), N7(H9AA), C41(H4BA)
3.d Idealised Me refined as rotating group:
 C4(HF,HG,HH), C42(H5BA,H6BA,H7BA), C19(H19A,H19B,H19C)
;
_shelx_res_checksum              50998
_olex2_submission_special_instructions 'No special instructions were received'