<i>tert</i>-Butyl (2<i>R</i>,4a<i>R</i>,5a<i>R</i>,11a<i>S</i>,12<i>R</i>,12a<i>R</i>)-8-[bis(<i>tert</i>-butoxycarbonyl)amino]-12-hydroxy-2-methoxy-2,10-dioxo-4,4a,5a,6,9,10,11,11a,12,12a-decahydro-2<i>H</i>-1,3,5-trioxa-6,7,9,11-tetraaza-2λ^5^-phosphatetracene-6-carboxylate methanol monosolvate monohydrate
Gainsford, Graeme J.; Clinch, Keith; Dixon, Rachel; Tiwari, Ashish; Acta Crystallographica Section E 68 (2012) o2250–o2251; doi:10.1107/S160053681202867X

data_2235353
_publ_section_title
;
 <i>tert</i>-Butyl
 (2<i>R</i>,4a<i>R</i>,5a<i>R</i>,11a<i>S</i>,12<i>R</i>,12a<i>R</i>)-8-[bis(<i>tert</i>-butoxycarbonyl)amino]-12-hydroxy-2-methoxy-2,10-dioxo-4,4a,5a,6,9,10,11,11a,12,12a-decahydro-2<i>H</i>-1,3,5-trioxa-6,7,9,11-tetraaza-2\l^5^-phosphatetracene-6-carboxylate
 methanol monosolvate monohydrate
;
_journal_coeditor_code           BH2437
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2250
_journal_page_last               o2251
_journal_paper_doi               10.1107/S160053681202867X
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C26 H40 N5 O13 P, C H4 O, H2 O'
_chemical_formula_moiety         'C26 H40 N5 O13 P, C H4 O, H2 O'
_chemical_formula_sum            'C27 H46 N5 O15 P'
_chemical_formula_weight         711.66
_chemical_name_systematic
;
<i>tert</i>-Butyl (2<i>R</i>,4a<i>R</i>,5a<i>R</i>,11a<i>S</i>,12<i>R</i>,
12a<i>R</i>)-8-[bis(<i>tert</i>-butoxycarbonyl)amino]-12-hydroxy-2-
methoxy-2,10-dioxo-4,4a,5a,6,9,10,11,11a,12,12a-decahydro-2<i>H</i>-1,3,5-
trioxa-6,7,9,11-tetraaza-2\l^5^-phosphatetracene-6-carboxylate
methanol monosolvate monohydrate
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.6435(4)
_cell_length_b                   15.9508(13)
_cell_length_c                   21.1764(8)
_cell_measurement_reflns_used    8356
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      73.6689
_cell_measurement_theta_min      2.7702
_cell_volume                     3595.2(4)
_computing_cell_refinement       'CrysAlis PRO (Oxford Diffraction, 2007)'
_computing_data_collection       'CrysAlis PRO (Oxford Diffraction, 2007)'
_computing_data_reduction        'CrysAlis PRO (Oxford Diffraction, 2007)'
_computing_molecular_graphics
'ORTEP in WinGX (Farrugia, 1999) and Mercury (Macrae <i>et al.</i>, 2008)'
_computing_publication_material
'SHELXL97 (Sheldrick, 2008) and PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 10.6501
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
'Oxford Diffraction SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0401
_diffrn_reflns_av_sigmaI/netI    0.0401
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            20603
_diffrn_reflns_theta_full        69.98
_diffrn_reflns_theta_max         69.98
_diffrn_reflns_theta_min         3.47
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.309
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85320
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrysAlis PRO; Oxford Diffraction, 2007)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.315
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1512
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.405
_refine_diff_density_min         -0.484
_refine_ls_abs_structure_details 'Flack (1983), 2985 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.02(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     452
_refine_ls_number_reflns         6796
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0430
_refine_ls_R_factor_gt           0.0376
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0524P)^2^+0.4160P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0920
_refine_ls_wR_factor_ref         0.0955
_reflns_number_gt                6210
_reflns_number_total             6796
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bh2437.cif
_cod_data_source_block           I
_cod_original_cell_volume        3595.2(3)
_cod_database_code               2235353
_cod_database_fobs_code          2235353