Bis[3-(trimethylsilyl)propyl] ethylenebisphosphonate, H~2~DTMSP[EBP]
McLauchlan, Craig C.; Ziegler, Amanda J.; Sosnowski, Cyndi R.; Herlinger, Albert W.; Acta Crystallographica Section C 63 (2007) o132–o134; doi:10.1107/S0108270106055818

data_2015818
_publ_section_title
;
 Bis[3-(trimethylsilyl)propyl] ethylenebisphosphonate, H~2~DTMSP[EBP]
;
_journal_coeditor_code           SQ3056
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o132
_journal_page_last               o134
_journal_paper_doi               10.1107/S0108270106055818
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C14 H36 O6 P2 Si2'
_chemical_formula_moiety         'C14 H36 O6 P2 Si2'
_chemical_formula_sum            'C14 H36 O6 P2 Si2'
_chemical_formula_weight         418.55
_chemical_melting_point          91.0(10)
_chemical_name_common
;
P,P'-di[3-(trimethylsilyl)-1-propyl]
ethylenebisphosphonic acid
;
_chemical_name_systematic
;
Bis[3-(trimethylsilyl)propyl] ethylenebisphosphonate
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.6865(3)
_cell_length_b                   11.0294(8)
_cell_length_c                   26.8912(13)
_cell_measurement_reflns_used    6010
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.4975
_cell_measurement_theta_min      3.7833
_cell_volume                     2279.8(2)
_computing_cell_refinement       'CrysAlis RED (Oxford, 2006)'
_computing_data_collection       'CrysAlis CCD (Oxford, 2006)'
_computing_data_reduction        'CrysAlis RED'
_computing_molecular_graphics    SHELXL97
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 15.9890
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Oxford Xcalibur3 CCD area-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  0.0255
_diffrn_reflns_av_sigmaI/netI    0.0239
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            10013
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.95
_diffrn_standards_decay_%        <1
_diffrn_standards_interval_count '50 frames'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.319
_exptl_absorpt_correction_T_max  0.948
_exptl_absorpt_correction_T_min  0.923
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
Analytical numerical absorption correction using a multifaceted crystal
model based on expressions derived by Clark & Reid (1995)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.219
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             904
_exptl_crystal_size_max          0.3874
_exptl_crystal_size_mid          0.2385
_exptl_crystal_size_min          0.2140
_refine_diff_density_max         0.403
_refine_diff_density_min         -0.283
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     113
_refine_ls_number_reflns         2598
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0449
_refine_ls_R_factor_gt           0.0327
_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^)+(0.0448P)^2^+0.9918P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0801
_refine_ls_wR_factor_ref         0.0869
_reflns_number_gt                2091
_reflns_number_total             2598
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sq3056.cif
_cod_data_source_block           I
_cod_database_code               2015818
_cod_database_fobs_code          2015818