Bis[3-(trimethylsilyl)propyl] methylenebisphosphonate
McLauchlan, Craig C.; Stepinski, Dominique C.; Herlinger, Albert W.; Acta Crystallographica Section E 60 (2004) o2232–o2234; doi:10.1107/S1600536804028028

data_2204607
_publ_section_title
;
 Bis[3-(trimethylsilyl)propyl] methylenebisphosphonate
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2232
_journal_page_last               o2234
_journal_paper_doi               10.1107/S1600536804028028
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          'C13 H34 O6 P2 Si2'
_chemical_formula_moiety         'C13 H34 O6 P2 Si2'
_chemical_formula_sum            'C13 H34 O6 P2 Si2'
_chemical_formula_weight         404.52
_chemical_melting_point          313.0(10)
_chemical_name_systematic
;
Bis[3-(trimethylsilyl)propyl] methylenebisphosphonate
;
_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                100.640(10)
_cell_angle_beta                 100.250(10)
_cell_angle_gamma                106.23(2)
_cell_formula_units_Z            2
_cell_length_a                   6.534(2)
_cell_length_b                   11.130(2)
_cell_length_c                   16.325(2)
_cell_measurement_reflns_used    3959
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.4232
_cell_measurement_theta_min      1.7559
_cell_volume                     1086.6(4)
_computing_cell_refinement
;
CrysAlis RED (Oxford Diffraction, 2004)
;
_computing_data_collection
;
CrysAlis CCD (Oxford Diffraction, 2004)
;
_computing_data_reduction
;
CrysAlis RED
;
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type
;
Oxford Diffraction Xcalibur3 diffractometer equipped with a CCD detector
;
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0463
_diffrn_reflns_av_sigmaI/netI    0.0556
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            10850
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         4.20
_diffrn_standards_decay_%        <1
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.332
_exptl_absorpt_correction_T_max  0.98329
_exptl_absorpt_correction_T_min  0.88844
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(Clark & Reid, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.236
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             436
_exptl_crystal_size_max          0.36465
_exptl_crystal_size_mid          0.13321
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.998
_refine_diff_density_min         -0.573
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.148
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     214
_refine_ls_number_reflns         4971
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.148
_refine_ls_R_factor_all          0.0815
_refine_ls_R_factor_gt           0.0607
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.1P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1591
_refine_ls_wR_factor_ref         0.1780
_reflns_number_gt                3556
_reflns_number_total             4971
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            br6168.cif
_cod_data_source_block           I
_cod_database_code               2204607
_cod_database_fobs_code          2204607