Exploring Gem-Dimethyl Effect in the Formation of Imine-Based Macrocycles and Cages
Madhu, Suresh; Rashmi, E.; Gonnade, Rajesh G.; Sanjayan, G. J.; New J. Chem. 41 (2017) 8721–8724; doi:10.1039/C7NJ02069D

data_7056455
_publ_section_title
;
 Exploring Gem-Dimethyl Effect in the Formation of Imine-Based Macrocycles
 and Cages
;
_journal_issue                   17
_journal_name_full               'New J. Chem.'
_journal_page_first              8721
_journal_page_last               8724
_journal_paper_doi               10.1039/C7NJ02069D
_journal_volume                  41
_journal_year                    2017
_chemical_formula_moiety         'C54 H60 N6, 1.5(C H3 C N)'
_chemical_formula_sum            'C57 H64.5 N7.5'
_chemical_formula_weight         854.65
_space_group_crystal_system      triclinic
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_space_group_name_Hall           '-P 1'
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_symmetry_space_group_name_Hall  '-P 1'
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_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-03-15 deposited with the CCDC.
2017-07-20 downloaded from the CCDC.
;
_cell_angle_alpha                102.170(5)
_cell_angle_beta                 92.478(7)
_cell_angle_gamma                98.250(4)
_cell_formula_units_Z            4
_cell_length_a                   16.593(2)
_cell_length_b                   17.657(2)
_cell_length_c                   17.872(3)
_cell_measurement_reflns_used    9551
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.26
_cell_measurement_theta_min      2.38
_cell_volume                     5050.9(12)
_computing_cell_refinement       'SAINT (Bruker, 2016)'
_computing_data_collection       'APEX3 (Bruker, 2016)'
_computing_data_reduction        'SAINT (Bruker, 2016)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Photon II CPAD Area Detector'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE Kappa Duo PHOTON II CPAD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multilayer mirrors'
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_av_R_equivalents  0.0322
_diffrn_reflns_av_unetI/netI     0.0196
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
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_diffrn_reflns_theta_max         28.243
_diffrn_reflns_theta_min         2.338
_diffrn_source                   'micro-focus sealed tube'
_diffrn_source_type              'Incoatech I\mS HB'
_exptl_absorpt_coefficient_mu    0.067
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_exptl_absorpt_correction_T_min  0.984
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS(BRUKER, 2016)'
_exptl_crystal_colour            COLOURLESS
_exptl_crystal_density_diffrn    1.124
_exptl_crystal_description       PLATE
_exptl_crystal_F_000             1836
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile'
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.070
_platon_squeeze_details
;
The unit cell contained two more molecules of acetonitrile which
have been treated as a diffuse contribution to the overall
scattering without specific atom positions by SQUEESE/PLATON
;
_refine_diff_density_max         0.400
_refine_diff_density_min         -0.227
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
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_refine_ls_number_reflns         24834
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_refine_ls_R_factor_all          0.0519
_refine_ls_R_factor_gt           0.0451
_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^)+(0.1000P)^2^+0.5447P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1430
_refine_ls_wR_factor_ref         0.1484
_reflns_Friedel_coverage         0.000
_reflns_number_gt                21423
_reflns_number_total             24834
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7nj02069d2.cif
_cod_data_source_block           1_sqd
_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 

2017-10-04
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_cell_volume        5051.2(11)
_cod_original_formula_moiety     '2(C54 H60 N6), 3(C H3 C N)'
_cod_original_formula_sum        'C114 H129 N15'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     1709.31
_cod_database_code               7056455
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.984
_shelx_estimated_absorpt_t_max   0.995
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              11788