Redetermined structure of methyl 3-{4,4-difluoro-2-[2-(methoxycarbonyl)ethyl]-1,3,5,7-tetramethyl-4-bora-3a,4a-diaza-s-indacen-6-yl}propionate
Schollmeyer, Dieter; Jochen, Matthias; Detert, Heiner; IUCrData 9 (2024) x240884–; doi:10.1107/S2414314624008848

data_1572657
_publ_section_title
;
 Redetermined structure of methyl
 3-{4,4-difluoro-2-[2-(methoxycarbonyl)ethyl]-1,3,5,7-tetramethyl-4-bora-3a,4a-diaza-s-indacen-6-yl}propionate
;
_journal_coeditor_code           HB4485
_journal_issue                   9
_journal_name_full               IUCrData
_journal_page_first              x240884
_journal_paper_doi               10.1107/S2414314624008848
_journal_volume                  9
_journal_year                    2024
_chemical_formula_iupac          'C21 H27 B F2 N2 O4'
_chemical_formula_moiety         'C21 H27 B F2 N2 O4'
_chemical_formula_sum            'C21 H27 B F2 N2 O4'
_chemical_formula_weight         420.25
_chemical_name_common
'3-[2'(2''-Methoxycarbonylethyl)-1',3',5',7'-tetramethyl-4',4'-difluoro-4'-bora-3a',4a'-diaza-s-indacen-6'-yl]propionic acid methyl ester'
_chemical_name_systematic
;Methyl
3-{4,4-difluoro-2-[2-(methoxycarbonyl)ethyl]-1,3,5,7-tetramethyl-4-bora-3a,4a-diaza-<i>s</i>-indacen-6-yl}propionate
;
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 108.251(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.9299(8)
_cell_length_b                   21.6278(17)
_cell_length_c                   8.2665(6)
_cell_measurement_reflns_used    6884
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.30
_cell_measurement_theta_min      2.59
_cell_volume                     2025.6(3)
_computing_cell_refinement
;
X-Area Recipe 1.36.0.0 (Stoe & Cie, 2020)
;
_computing_data_collection
;
X-Area WinXpose 2.0.22.0 (Stoe & Cie, 2020)
;
_computing_data_reduction
;
X-Area Integrate 1.77.0.0 (Stoe & Cie, 2020)
;
_computing_molecular_graphics
;
PLATON (Spek, 2020)
;
_computing_structure_refinement
;
<i>SHELXL2018/3</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT2014</i> (Shelxdrick, 2015a)
;
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Stoe IPDS 2T'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0523
_diffrn_reflns_av_unetI/netI     0.0698
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            9943
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.165
_diffrn_reflns_theta_min         2.604
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_exptl_absorpt_coefficient_mu    0.106
_exptl_absorpt_correction_T_max  0.9954
_exptl_absorpt_correction_T_min  0.9852
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
(XRED32; Stoe & Cie, 2020)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.378
_exptl_crystal_description       plate
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.498
_refine_diff_density_min         -0.482
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     277
_refine_ls_number_reflns         4863
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.1757
_refine_ls_R_factor_gt           0.0895
_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^)+(0.0569P)^2^+5.4328P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1824
_refine_ls_wR_factor_ref         0.2379
_reflns_number_gt                2663
_reflns_number_total             4863
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            hb4485.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1572657
_shelx_estimated_absorpt_t_min   0.979
_shelx_estimated_absorpt_t_max   0.996
_shelx_hkl_checksum              9005
_shelx_res_checksum              34350