Two closely related {4-[(<i>N</i>-substituted amino)(diethoxyphosphoryl)methyl]phenyl}boronic acids
Zhang, Rui; Zhang, Yundi; Ge, Chunhua; Miao, Jinpeng; Zhang, Xiangdong; Acta Crystallographica Section C 73 (2017) 57–60; doi:10.1107/S2053229616019707

data_2020702
_publ_section_title
;
 Two closely related {4-[(<i>N</i>-substituted
 amino)(diethoxyphosphoryl)methyl]phenyl}boronic acids
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              57
_journal_page_last               60
_journal_paper_doi               10.1107/S2053229616019707
_journal_volume                  73
_journal_year                    2017
_chemical_formula_iupac          'C17 H22 B N2 O7 P'
_chemical_formula_moiety         'C17 H22 B N2 O7 P'
_chemical_formula_sum            'C17 H22 B N2 O7 P'
_chemical_formula_weight         408.14
_chemical_name_systematic
;
{4-[(Diethoxyphosphoryl)(4-nitroanilino)methyl]phenyl}boronic acid
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   10.2590(8)
_cell_length_b                   14.5721(14)
_cell_length_c                   27.577(3)
_cell_measurement_reflns_used    3802
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.29
_cell_measurement_theta_min      3.16
_cell_volume                     4122.6(7)
_computing_cell_refinement
;
SAINT (Bruker, 2010)
;
_computing_data_collection
;
APEX2 (Bruker, 2010)
;
_computing_data_reduction
;
SAINT (Bruker, 2010)
;
_computing_molecular_graphics
;
SHELXTL (Bruker, 2010)
;
_computing_publication_material
;
SHELXTL (Bruker, 2010)
;
_computing_structure_refinement
;
SHELXL2016 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.981
_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  0.0560
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            15530
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.370
_diffrn_reflns_theta_min         3.162
_exptl_absorpt_coefficient_mu    0.173
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.315
_exptl_crystal_description       sheet
_exptl_crystal_F_000             1712
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.608
_refine_diff_density_min         -0.326
_refine_ls_extinction_coef       0.0023(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2016 (Sheldrick, 2015)
;
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     265
_refine_ls_number_reflns         3726
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.1170
_refine_ls_R_factor_gt           0.0599
_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^)+(0.0813P)^2^+5.3769P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1424
_refine_ls_wR_factor_ref         0.1968
_reflns_number_gt                2312
_reflns_number_total             3726
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            eg3210sup1.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 2020701--2020702.cif.'
_cod_original_cell_volume        4122.6(6)
_cod_database_code               2020702
_cod_database_fobs_code          2020702
_shelx_estimated_absorpt_t_min   0.966
_shelx_estimated_absorpt_t_max   0.983
_shelx_hkl_checksum              57418
_shelx_res_checksum              5246