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_4029500
_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            'C37 H44 N P'
_chemical_formula_weight         533.74
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 96.439(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.6810(16)
_cell_length_b                   21.154(3)
_cell_length_c                   19.294(2)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.3
_cell_measurement_theta_min      1.8
_cell_volume                     6765.3(14)
_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 0.933
_diffrn_measured_fraction_theta_max 0.933
_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  0.1777
_diffrn_reflns_av_sigmaI/netI    0.1899
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            54010
_diffrn_reflns_theta_full        26.30
_diffrn_reflns_theta_max         26.30
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    0.104
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.048
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             2303
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.301
_refine_diff_density_min         -0.192
_refine_diff_density_rms         0.042
_refine_ls_extinction_coef       0.0051(5)
_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   0.712
_refine_ls_hydrogen_treatment    calculated
_refine_ls_matrix_type           full
_refine_ls_number_parameters     704
_refine_ls_number_reflns         12809
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.712
_refine_ls_R_factor_all          0.2569
_refine_ls_R_factor_gt           0.0688
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1061P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1628
_refine_ls_wR_factor_ref         0.2426
_reflns_number_gt                2675
_reflns_number_total             12809
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo901942u_si_003.cif
_cod_data_source_block           cmpd2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from
2011-04-26.

'_exptl_absorpt_correction_type' value 'None' changed to
'none' according to
/usr/data/users/saulius/automatic-downloads/retrospective/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Updated bibliographic information.

 Antanas Vaitkus,
 2019-10-01
;
_cod_original_cell_volume        6765.3(13)
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_database_code               4029500