(9<i>H</i>-Fluoren-9-yl)methyl <i>N</i>-{(2<i>R</i>,3<i>R</i>,4<i>S</i>)-4-hydroxy-2-[(2<i>S</i>,5<i>R</i>)-2-isopropyl-5-methylcyclohexyloxy]-5-oxooxolan-3-yl}carbamate propan-2-ol 0.334-solvate
Gainsford, Graeme J.; Luxenburger, Andreas; Acta Crystallographica Section E 68 (2012) o403–o404; doi:10.1107/S1600536811055139

data_2233411
_publ_section_title
;
 (9<i>H</i>-Fluoren-9-yl)methyl
 <i>N</i>-{(2<i>R</i>,3<i>R</i>,4<i>S</i>)-4-hydroxy-2-[(2<i>S</i>,5<i>R</i>)-2-isopropyl-5-methylcyclohexyloxy]-5-oxooxolan-3-yl}carbamate
 propan-2-ol 0.334-solvate
;
_journal_coeditor_code           CV5219
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o403
_journal_page_last               o404
_journal_paper_doi               10.1107/S1600536811055139
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C29 H35 N O6, 0.334C3 H8 O'
_chemical_formula_moiety         'C29 H35 N O6, 0.334(C3 H8 O)'
_chemical_formula_sum            'C30 H37.667 N O6.333'
_chemical_formula_weight         513.64
_chemical_name_systematic
;
(9<i>H</i>-Fluoren-9-yl)methyl <i>N</i>-{(2<i>R</i>,3<i>R</i>,4<i>S</i>)-
4-hydroxy-2-[(2<i>S</i>,5<i>R</i>)-2-isopropyl-5-methylcyclohexyloxy]-5-
oxooxolan-3-yl}carbamate propan-2-ol 0.334-solvate
;
_space_group_IT_number           1
_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                98.495(7)
_cell_angle_beta                 92.109(7)
_cell_angle_gamma                91.120(6)
_cell_formula_units_Z            2
_cell_length_a                   5.1786(2)
_cell_length_b                   15.3176(5)
_cell_length_c                   20.3554(14)
_cell_measurement_reflns_used    11033
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      71.6
_cell_measurement_theta_min      6.1
_cell_volume                     1595.36(14)
_computing_cell_refinement
;
<i>FSProcess</i> in <i>PROCESS-AUTO</i> (Rigaku, 1998)
;
_computing_data_collection       'CrystalClear (Rigaku, 2005)'
_computing_data_reduction
;
<i>FSProcess</i> in <i>PROCESS-AUTO</i> (Rigaku, 1998)
;
_computing_molecular_graphics
;
ORTEP in WinGX (Farrugia, 1999) and Mercury (Macrae <i>et al.</i>,
2008)
;
_computing_publication_material
;
SHELXL97 (Sheldrick, 2008), PLATON (Spek, 2009) and HYDROGEN
(Nardelli, 1999)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.853
_diffrn_measured_fraction_theta_max 0.853
_diffrn_measurement_device_type
;
Rigaku Spider
;
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator
;
Rigaku VariMax-HF Confocal Optical System
;
_diffrn_radiation_source
;
 Rigaku MM007 rotating anode
;
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.086
_diffrn_reflns_av_sigmaI/netI    0.101
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            7392
_diffrn_reflns_theta_full        62.38
_diffrn_reflns_theta_max         62.38
_diffrn_reflns_theta_min         8.94
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.604
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.667
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.069
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             551
_exptl_crystal_size_max          0.67
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_platon_squeeze_details
;
TITL al22                   R = 0.18
CELL    5.1786   15.3176   20.3554     98.50     92.11     91.12
SPGR P1
C101 0.943 0.507 0.034 !       3.05 eA-3
C102 0.862 0.449 0.095 !       2.54 eA-3
C103 0.758 0.063 0.660 !       2.05 eA-3
C104 0.290 0.356 0.889 !       1.65 eA-3
C105 0.090 0.385 0.092 !       1.58 eA-3
C106 0.781 0.160 0.640 !       1.53 eA-3
C107 0.981 0.081 0.707 !       1.51 eA-3
C108 0.144 0.210 0.891 !       1.37 eA-3
C109 0.304 0.253 0.878 !       1.29 eA-3
C110 0.849 0.496 0.160 !       1.22 eA-3
C111 0.840 0.519 0.140 !       1.20 eA-3
C112 0.060 0.346 0.922 !       1.18 eA-3
Q113 0.542 0.144 0.738 !       1.06 eA-3
C114 0.448 0.217 0.827 !       1.02 eA-3
Q115 0.493 0.892 0.538 !       0.94 eA-3
C116 0.745 0.014 0.703 !       0.94 eA-3
C117 0.562 1.007 0.693 !       0.85 eA-3
Q118 0.561 0.925 0.514 !       0.85 eA-3
C119 0.748 0.110 0.702 !       0.85 eA-3
C120 0.604 0.035 0.598 !       0.83 eA-3
C121 0.621 0.897 0.736 !       0.80 eA-3
C122 0.994 0.347 0.217 !       0.75 eA-3
C123 0.752 0.902 0.542 !       0.74 eA-3
C124 0.849 0.064 0.736 !       0.74 eA-3
Q125 0.385 0.194 0.776 !       0.73 eA-3
C126 0.573 0.247 0.861 !       0.70 eA-3
C127 0.965 0.181 0.825 !       0.64 eA-3
Q128 0.190 0.043 0.894 !       0.63 eA-3
C129 1.016 0.971 0.829 !       0.63 eA-3
Q130 0.135 0.888 0.058 !       0.59 eA-3
Q131 0.050 0.067 0.925 !       0.59 eA-3
Q132 0.409 0.486 0.893 !       0.58 eA-3
Q133 0.216 0.858 0.109 !       0.57 eA-3
Q134 0.647 0.220 0.503 !       0.56 eA-3
Q135 0.897 0.198 0.436 !       0.56 eA-3
Q136 0.969 0.325 0.575 !       0.55 eA-3
Q137 0.285 0.079 0.940 !       0.54 eA-3
Q138 0.054 0.754 0.106 !       0.54 eA-3
Q139 1.000 0.408 0.249 !       0.54 eA-3
Q140 0.399 0.092 0.888 !       0.53 eA-3
Q141 0.824 0.602 0.077 !       0.53 eA-3
Q142 0.243 0.828 0.095 !       0.53 eA-3
Q143 0.203 0.640 0.451 !       0.53 eA-3
Q144 0.142 0.220 0.470 !       0.53 eA-3
Q145 0.550 0.021 0.501 !       0.53 eA-3
Q146 0.316 0.604 0.487 !       0.52 eA-3
Q147 0.504 0.530 0.391 !       0.52 eA-3
Q148 0.641 0.520 0.030 !       0.51 eA-3
Q149 0.439 0.958 0.468 !       0.51 eA-3
Q150 0.237 0.258 0.080 !       0.50 eA-3
Q151 0.086 0.735 0.158 !       0.50 eA-3
;
_refine_diff_density_max         0.406
_refine_diff_density_min         -0.332
_refine_ls_extinction_coef       0.0101(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     673
_refine_ls_number_reflns         7392
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.1188
_refine_ls_R_factor_gt           0.0952
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1783P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2311
_refine_ls_wR_factor_ref         0.2605
_reflns_number_gt                5189
_reflns_number_total             7392
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            cv5219.cif
_cod_data_source_block           I
_cod_database_code               2233411
_cod_database_fobs_code          2233411