Scope and limitations of the base-catalyzed phospha-peterson P=C bond-forming reaction.
Yam, Mandy; Chong, Jonathan H.; Tsang, Chi-Wing; Patrick, Brian O.; Lam, Anita E.; Gates, Derek P.; Inorganic chemistry 45 (2006) 5225–5234; doi:10.1021/ic060236p

data_4350262
_publ_section_title
;
 Scope and limitations of the base-catalyzed phospha-peterson P=C
 bond-forming reaction.
;
_journal_issue                   13
_journal_name_full               'Inorganic chemistry'
_journal_page_first              5225
_journal_page_last               5234
_journal_paper_doi               10.1021/ic060236p
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C50 H58 O P2'
_chemical_formula_weight         736.90
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 122.037(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.447(2)
_cell_length_b                   15.2803(9)
_cell_length_c                   13.5330(11)
_cell_measurement_reflns_used    11096
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.87
_cell_measurement_theta_min      2.67
_cell_volume                     3934.9(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 11.76
_diffrn_measured_fraction_theta_full 0.458
_diffrn_measured_fraction_theta_max 0.458
_diffrn_measurement_device_type  'Rigaku/ADSC CCD'
_diffrn_measurement_method       'area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0530
_diffrn_reflns_av_sigmaI/netI    0.0608
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            4458
_diffrn_reflns_theta_full        27.87
_diffrn_reflns_theta_max         27.87
_diffrn_reflns_theta_min         2.67
_exptl_absorpt_coefficient_mu    0.149
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.791
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.244
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1584
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.371
_refine_diff_density_min         -0.257
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     291
_refine_ls_number_reflns         4458
_refine_ls_number_restraints     91
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0616
_refine_ls_R_factor_gt           0.0416
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0593P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1037
_refine_ls_wR_factor_ref         0.1117
_reflns_number_gt                3355
_reflns_number_total             4458
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060236psi20060211_073220.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
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The following automatic conversions were performed:

data item '_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0593P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. A new data item '_refine_ls_weighting_details' was
created with the value set to
'w=1/[\s^2^(Fo^2^)+(0.0593P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        3934.8(5)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4350262