C,C-Diacetylenic Phosphaalkenes as Heavy Diethynylethene Analogues
Öberg, Elisabet; Schäfer, Bernhard; Geng, Xue-Li; Pettersson, Jenny; Hu, Qi; Kritikos, Mikael; Rasmussen, Torben; Ott, Sascha; The Journal of Organic Chemistry 74 (2009) 9265–9273; doi:10.1021/jo901942u

data_4028963
_publ_section_title
;
 C,C-Diacetylenic Phosphaalkenes as Heavy Diethynylethene Analogues
;
_journal_coden_ASTM              JOCEAH
_journal_issue                   24
_journal_name_full               'The Journal of Organic Chemistry'
_journal_page_first              9265
_journal_page_last               9273
_journal_paper_doi               10.1021/jo901942u
_journal_volume                  74
_journal_year                    2009
_chemical_formula_sum            'C35 H38.5 N O2 P'
_chemical_formula_weight         536.14
_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                111.142(15)
_cell_angle_beta                 93.977(15)
_cell_angle_gamma                92.936(15)
_cell_formula_units_Z            2
_cell_length_a                   8.7338(10)
_cell_length_b                   13.3618(17)
_cell_length_c                   14.4726(19)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.3
_cell_measurement_theta_min      2.6
_cell_volume                     1566.2(4)
_computing_cell_refinement       'IPDS Software, Stoe & Cie (1997)'
_computing_data_collection       'IPDS Software, by Stoe & Cie (1997)'
_computing_data_reduction        'IPDS Software,  Stoe & Cie (1997)'
_computing_molecular_graphics
'PLATON99 (Spek, 2000), DIAMOND (Brandenburg, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.922
_diffrn_measured_fraction_theta_max 0.922
_diffrn_measurement_device_type  'STOE IPDS'
_diffrn_measurement_method       'phi oscillation'
_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  0.0848
_diffrn_reflns_av_sigmaI/netI    0.1158
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            12404
_diffrn_reflns_theta_full        26.18
_diffrn_reflns_theta_max         26.18
_diffrn_reflns_theta_min         2.61
_exptl_absorpt_coefficient_mu    0.118
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.137
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             573
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.366
_refine_diff_density_min         -0.247
_refine_diff_density_rms         0.040
_refine_ls_extinction_coef       0.021(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.826
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     348
_refine_ls_number_reflns         5809
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.826
_refine_ls_R_factor_all          0.1279
_refine_ls_R_factor_gt           0.0523
_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^)+(0.0705P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1156
_refine_ls_wR_factor_ref         0.1445
_reflns_number_gt                2571
_reflns_number_total             5809
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo901942usup2.cif
_cod_data_source_block           cmpd1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'None' changed to 'none'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

 Updated bibliographic information.

 Antanas Vaitkus,
 2019-10-01
;
_cod_original_cell_volume        1566.2(3)
_cod_original_formula_sum        'C35 H38.50 N O2 P'
_cod_database_code               4028963