Crystal structure of a methanol solvate of a macrocycle bearing two flexible side-arms
Amrhein, Felix; Schwarzer, Anke; Mazik, Monika; Acta Crystallographica Section E 77 (2021) 233–236; doi:10.1107/S2056989021001067

data_2243746
_publ_section_title
;
 Crystal structure of a methanol solvate of a macrocycle bearing two
 flexible side-arms
;
_journal_coeditor_code           ZQ2258
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              233
_journal_page_last               236
_journal_paper_doi               10.1107/S2056989021001067
_journal_volume                  77
_journal_year                    2021
_chemical_formula_iupac          'C52 H72 N8 O4, 2C H4 O'
_chemical_formula_moiety         'C52 H72 N8 O4, 2(C H4 O)'
_chemical_formula_sum            'C54 H80 N8 O6'
_chemical_formula_weight         937.26
_chemical_name_systematic
;Di-<i>tert</i>-butyl
<i>N</i>,<i>N</i>'-{[13,15,28,30,31,33-hexaethyl-3,10,18,25,32,34-hexaazapentacyclo[25.3.1.1^5,8^.1^12,16^.1^20,23^]tetratriaconta-1(31),3,5,7,9,12(33),13,15,18,20,22,24,27,29-tetradecaene-14,29-diyl]bis(methylene)}dicarbamate methanol disolvate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 102.800(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.8395(9)
_cell_length_b                   20.0443(19)
_cell_length_c                   9.6347(9)
_cell_measurement_reflns_used    4018
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.14
_cell_measurement_theta_min      2.56
_cell_volume                     2606.3(4)
_computing_cell_refinement
;
SAINT (Bruker, 2007)
;
_computing_data_collection
;
APEX2 (Bruker, 2007)
;
_computing_data_reduction
;
SAINT (Bruker, 2007)
;
_computing_molecular_graphics
;
XP (Sheldrick, 2008)
;
_computing_publication_material
;
<i>WinGX</i> (Farrugia, 2012), <i>publCIF</i> (Westrip, 2010)
and <i>shelXle</i>
(H\"ubschle <i>et al.</i>,  2011)
;
_computing_structure_refinement
;
<i>SHELXL2018/3</i> (Sheldrick, 2015)
;
_computing_structure_solution
;
SIR2014 (Burla <i>et al.</i>, 2015)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0361
_diffrn_reflns_av_unetI/netI     0.0236
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            35355
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_min         3.076
_exptl_absorpt_coefficient_mu    0.078
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.194
_exptl_crystal_description       piece
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.310
_exptl_crystal_size_min          0.210
_refine_diff_density_max         0.323
_refine_diff_density_min         -0.241
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         5099
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0503
_refine_ls_R_factor_gt           0.0384
_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^)+(0.0490P)^2^+1.1359P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0951
_refine_ls_wR_factor_ref         0.1030
_reflns_number_gt                4185
_reflns_number_total             5099
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            zq2258sup1.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2243746
_cod_database_fobs_code          2243746
_shelx_estimated_absorpt_t_min   0.973
_shelx_estimated_absorpt_t_max   0.984
_shelx_hkl_checksum              574
_shelx_res_checksum              6231