Camphene-derived primary and hydroxymethyl phosphines
Berrigan, Rebecca A.; Russell, Douglas K.; Henderson, William; Leach, Meto T.; Nicholson, Brian K.; Woodward, Gary; Harris, Christopher; New Journal of Chemistry 25 (2001) 322–; doi:10.1039/b006252i

data_7051032
_publ_section_title
;
 Camphene-derived primary and hydroxymethyl phosphines
;
_journal_issue                   2
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              322
_journal_paper_doi               10.1039/b006252i
_journal_volume                  25
_journal_year                    2001
_chemical_formula_sum            'C13 H26 Cl O3 P'
_chemical_formula_weight         296.76
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 92.54(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.504(7)
_cell_length_b                   7.561(5)
_cell_length_c                   12.142(3)
_cell_measurement_reflns_used    18
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      5
_cell_volume                     1513.7(12)
_computing_cell_refinement       SHELXTL
_computing_data_collection       SHELXTL
_computing_data_reduction        SHELXTL
_computing_molecular_graphics    PLUTO
_computing_publication_material  SHELX97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1993)'
_computing_structure_solution    SHELX97
_diffrn_ambient_temperature      130(2)
_diffrn_measurement_device       'Nicolet R3 four-circle'
_diffrn_measurement_method       'omega scans'
_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  0.0272
_diffrn_reflns_av_sigmaI/netI    0.0688
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2798
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.47
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.357
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.302
_exptl_crystal_description       needle
_exptl_crystal_F_000             640
_exptl_crystal_size_max          0.57
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.345
_refine_diff_density_min         -0.216
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.023
_refine_ls_goodness_of_fit_obs   1.104
_refine_ls_hydrogen_treatment    RIDING
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         2657
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_restrained_S_obs      1.104
_refine_ls_R_factor_all          0.0927
_refine_ls_R_factor_obs          0.0467
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0486P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1100
_refine_ls_wR_factor_obs         0.0936
_reflns_number_observed          1706
_reflns_number_total             2657
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b006252i.txt
_cod_data_source_block           camp
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0486P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0486P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7051032