<i>tert</i>-Butyl <i>N</i>-(phosphinoyloxy)carbamate
Blatch, Alexandrea J.; Howard, Judith A. K.; Probert, Michael R.; Smethurst, Christian A.; Whiting, Andrew; Acta Crystallographica Section E 62 (2006) o5346–o5348; doi:10.1107/S1600536806044783

data_2211034
_publ_section_title
;
 <i>tert</i>-Butyl <i>N</i>-(phosphinoyloxy)carbamate
;
_journal_coeditor_code           HB2179
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o5346
_journal_page_last               o5348
_journal_paper_doi               10.1107/S1600536806044783
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          'C17 H20 N O4 P'
_chemical_formula_moiety         'C17 H20 N O4 P'
_chemical_formula_sum            'C17 H20 N O4 P'
_chemical_formula_weight         333.31
_chemical_name_common
N-butoxycarbonyl-diphenylphosphinyl-hydroxylamine
_chemical_name_systematic
;
tert-Butyl N-(phosphinoyloxy)carbamate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                101.100(10)
_cell_angle_beta                 96.770(10)
_cell_angle_gamma                92.930(10)
_cell_formula_units_Z            6
_cell_length_a                   12.1810(10)
_cell_length_b                   13.7340(10)
_cell_length_c                   16.5320(10)
_cell_measurement_reflns_used    5811
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      34.36
_cell_measurement_theta_min      2.18
_cell_volume                     2687.3(4)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL (Bruker, 2003)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Bruker, 2001)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.843
_diffrn_measured_fraction_theta_max 0.753
_diffrn_measurement_device_type  'Bruker SMART CCD 6K'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0398
_diffrn_reflns_av_sigmaI/netI    0.0317
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            11843
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         1.52
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.171
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.236
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.548
_refine_diff_density_min         -0.534
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     652
_refine_ls_number_reflns         11796
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.0568
_refine_ls_R_factor_gt           0.0434
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0824P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1161
_refine_ls_wR_factor_ref         0.1253
_reflns_number_gt                9155
_reflns_number_total             11796
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb2179.cif
_cod_data_source_block           I
_cod_original_cell_volume        2687.3(3)
_cod_database_code               2211034
_cod_database_fobs_code          2211034