Bis[5-methoxy-2-(methoxycarbonyl)phenyl] methylphosphonate
Hussain, Saghir; Deli, Yang; Parveen, Shagufta; Hao, Xin; Zhu, Changjin; Acta Crystallographica Section E 70 (2014) o269–; doi:10.1107/S1600536814002542

data_2239385
_publ_section_title
;
 Bis[5-methoxy-2-(methoxycarbonyl)phenyl] methylphosphonate
;
_journal_coeditor_code           BH2491
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o269
_journal_paper_doi               10.1107/S1600536814002542
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          'C19 H21 O9 P'
_chemical_formula_moiety         'C19 H21 O9 P'
_chemical_formula_sum            'C19 H21 O9 P'
_chemical_formula_weight         424.33
_chemical_name_systematic
;
Bis[5-methoxy-2-(methoxycarbonyl)phenyl] methylphosphonate
;
_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                70.774(9)
_cell_angle_beta                 77.800(9)
_cell_angle_gamma                84.172(10)
_cell_formula_units_Z            2
_cell_length_a                   7.852(2)
_cell_length_b                   10.616(3)
_cell_length_c                   12.200(3)
_cell_measurement_reflns_used    3814
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      31.507
_cell_measurement_theta_min      2.249
_cell_volume                     938.0(4)
_computing_cell_refinement       'CrystalClear (Rigaku, 2008)'
_computing_data_collection       'CrystalClear (Rigaku, 2008)'
_computing_data_reduction        'CrystalClear (Rigaku, 2008)'
_computing_molecular_graphics
;
CrystalStructure (Rigaku, 2008) and <i>DIAMOND</i> (Brandenburg,
1999)
;
_computing_publication_material  'CrystalStructure (Rigaku, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Rigaku AFC10/Saturn724+'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0278
_diffrn_reflns_av_sigmaI/netI    0.0383
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13574
_diffrn_reflns_theta_full        31.00
_diffrn_reflns_theta_max         31.00
_diffrn_reflns_theta_min         2.25
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.199
_exptl_absorpt_correction_T_max  0.9547
_exptl_absorpt_correction_T_min  0.8898
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrystalClear; Rigaku, 2008)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.502
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             444
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.380
_refine_diff_density_min         -0.496
_refine_ls_extinction_coef       0.018(2)
_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   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     268
_refine_ls_number_reflns         5875
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0476
_refine_ls_R_factor_gt           0.0396
_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^)+(0.0463P)^2^+0.36P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0972
_refine_ls_wR_factor_ref         0.1024
_reflns_number_gt                5141
_reflns_number_total             5875
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bh2491sup1.cif
_cod_data_source_block           I
_cod_database_code               2239385
_cod_database_fobs_code          2239385