Synthesis and crystal structure of peptide dimethyl biphenyl hybrid C~52~H~60~N~6~O~10~·0.25H~2~O
Nguyen, Xuan Tu; Le, Thuy Quynh; Bui Thi, Tra My; Mac, Dinh Hung; Bui, Thai Thanh Thu; Acta Crystallographica Section E 76 (2020) 1675–1678; doi:10.1107/S2056989020012931

data_2243603
_publ_section_title
;
 Synthesis and crystal structure of peptide dimethyl biphenyl hybrid
 C~52~H~60~N~6~O~10~&#x00B7;0.25H~2~O
;
_journal_coeditor_code           VM2240
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1675
_journal_page_last               1678
_journal_paper_doi               10.1107/S2056989020012931
_journal_volume                  76
_journal_year                    2020
_chemical_absolute_configuration R
_chemical_formula_iupac          'C52 H60 N6 O10, 0.25H2 O'
_chemical_formula_moiety         'C52 H60 N6 O10, 0.25(H2 O)'
_chemical_formula_sum            'C52 H60.5 N6 O10.25'
_chemical_formula_weight         933.56
_chemical_name_systematic
'Dimethyl 2,2'-[((2<i>S</i>,2'<i>S</i>)-2,2'-{[(2<i>S</i>,2'<i>S</i>)-1,1'-(6,6'-dimethyl-[1,1'-biphenyl]-2,2'-dicarbonyl)bis(pyrrolidine-1,2-diyl-2-carbonyl)]bis(azanediyl)}bis(3-phenylpropanoyl))bis(azanediyl)](2<i>S</i>,2'<i>S</i>)-dipropionate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 99.999(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.505(3)
_cell_length_b                   12.3814(12)
_cell_length_c                   14.6346(14)
_cell_measurement_reflns_used    9371
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      25.747
_cell_measurement_theta_min      2.792
_cell_volume                     4908.1(9)
_computing_cell_refinement
;
SAINT (Bruker, 2013)
;
_computing_data_collection
;
APEX22 (Bruker 2013)
;
_computing_data_reduction
;
SAINT (Bruker, 2013)
;
_computing_molecular_graphics
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
ShelXL (Sheldrick, 2015b)
;
_computing_structure_solution
;
ShelXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 Quest CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0619
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            84318
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.747
_diffrn_reflns_theta_min         2.792
_exptl_absorpt_coefficient_mu    0.089
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.7130
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS-; Bruker, 2013)
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_density_diffrn    1.263
_exptl_crystal_description       needle
_exptl_crystal_F_000             1986
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.276
_refine_diff_density_min         -0.157
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 3323 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons et al., 2013)
;
_refine_ls_abs_structure_Flack   -0.1(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     693
_refine_ls_number_reflns         9371
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0520
_refine_ls_R_factor_gt           0.0381
_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^)+(0.0359P)^2^+2.1291P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0807
_refine_ls_wR_factor_ref         0.0862
_reflns_number_gt                7959
_reflns_number_total             9371
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            vm2240sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        4908.2(8)
_cod_original_formula_sum        'C52 H60.50 N6 O10.25'
_cod_database_code               2243603