5,5-Dimethyl-2-(naphthalen-1-yloxy)-1,3,2-dioxaphosphinane 2-oxide
Li, Zheng-Qiu; Sheng, Xi-Jun; Zuo, Na; Ren, Qing-Yun; He, Hong-Wu; Acta Crystallographica Section E 62 (2006) o3501–o3502; doi:10.1107/S1600536806028431

data_2209754
_publ_section_title
;
 5,5-Dimethyl-2-(naphthalen-1-yloxy)-1,3,2-dioxaphosphinane 2-oxide
;
_journal_coeditor_code           BI2042
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3501
_journal_page_last               o3502
_journal_paper_doi               10.1107/S1600536806028431
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          'C15 H17 O4 P'
_chemical_formula_moiety         'C15 H17 O4 P'
_chemical_formula_sum            'C15 H17 O4 P'
_chemical_formula_weight         292.26
_chemical_melting_point          395
_chemical_name_systematic
;
5,5-Dimethyl-2-(naphthalen-1-yloxy)-1,3,2-dioxaphosphinane 2-oxide
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 99.834(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   6.6577(11)
_cell_length_b                   9.2835(15)
_cell_length_c                   12.1075(19)
_cell_measurement_reflns_used    3167
_cell_measurement_temperature    292(2)
_cell_measurement_theta_max      27.05
_cell_measurement_theta_min      2.78
_cell_volume                     737.3(2)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Bruker, 1997)'
_diffrn_ambient_temperature      292(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker SMART CCD'
_diffrn_measurement_method       '\f and \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  0.0166
_diffrn_reflns_av_sigmaI/netI    0.0302
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5570
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.71
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.196
_exptl_absorpt_correction_T_max  0.9807
_exptl_absorpt_correction_T_min  0.9618
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.316
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             308
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.337
_refine_diff_density_min         -0.132
_refine_ls_abs_structure_details 'Flack (1983), 1483 Friedel pairs'
_refine_ls_abs_structure_Flack   0.05(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     183
_refine_ls_number_reflns         3257
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.0516
_refine_ls_R_factor_gt           0.0480
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0573P)^2^+0.0777P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1130
_refine_ls_wR_factor_ref         0.1156
_reflns_number_gt                3015
_reflns_number_total             3257
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bi2042.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2209754
_cod_database_fobs_code          2209754