C~38~H~54~N~3~O~9~P, a New Compound in Diazadihydrophosphinine Chemistry
García-Granda, S.; Santiago-García, R.; Bieger, K.; Acta Crystallographica Section C 52 (1996) 2857–2859; doi:10.1107/S0108270196007755

data_2005644
_publ_section_title
;
 C~38~H~54~N~3~O~9~P, a New Compound in Diazadihydrophosphinine
 Chemistry
;
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              2857
_journal_page_last               2859
_journal_paper_doi               10.1107/S0108270196007755
_journal_volume                  52
_journal_year                    1996
_chemical_formula_sum            'C38 H54 N3 O9 P'
_chemical_formula_weight         727.81
_chemical_melting_point          513.15
_chemical_name_systematic
;
 4-^t^butyl-1-cyclohexyl-2-diisopropylamino-6-(4-methoxyphenyl)-2-[4-methoxy-
 2,3,4-tris(methoxycarbonyl)-5-oxo-2-cyclopentenyliden]-1,2-dihydro-1,3,2-
diazaphosphinine.
;
_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'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 113.18(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.846(9)
_cell_length_b                   38.204(9)
_cell_length_c                   11.421(9)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      10
_cell_measurement_theta_min      5
_cell_volume                     3949(5)
_computing_cell_refinement       'CRYSDA (Beurskens et al., 1992)'
_computing_data_collection
'Diffractometer Control Software (Enraf-Nonius, 1994)'
_computing_data_reduction        'REFLEX (local program)'
_computing_molecular_graphics    'EUCLID (Spek, 1982)'
_computing_publication_material  SHELXL93
_computing_structure_refinement  SHELXL93
_computing_structure_solution    DIRDIF
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf-Nonius CAD4 Diffractometer'
_diffrn_measurement_method       \w-2\q
_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  0.083
_diffrn_reflns_av_sigmaI/netI    0.3264
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
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_diffrn_reflns_limit_k_min       0
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_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6056
_diffrn_reflns_theta_max         23.00
_diffrn_reflns_theta_min         1.07
_diffrn_standards_decay_%        4.24
_diffrn_standards_interval_count 200
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.125
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.297
_exptl_absorpt_correction_type
'empirical (XABS2: Parkin, Moezzi & Hope, 1995)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.224
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1560
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.20
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_refine_diff_density_max         0.270
_refine_diff_density_min         -0.304
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    'H atoms riding, with isotropic common U'
_refine_ls_matrix_type           full
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_refine_ls_R_factor_all          0.3048
_refine_ls_R_factor_obs          0.0580
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0761P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2329
_refine_ls_wR_factor_obs         0.1269
_reflns_number_observed          1742
_reflns_number_total             5469
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            kh1100.cif
_cod_data_source_block           kb36
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_chemical_melting_point' value '240\%C' was changed to '513.15' - it
was converted from degrees Celsius(C) to
Kelvins(K).

'_symmetry_cell_setting' value 'Monoclinic' changed to
'monoclinic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

'_geom_bond_publ_flag'
value 'Yes' changed to 'yes' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (28
times).

'_geom_angle_publ_flag' value 'Yes' changed to 'yes'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (43
times).

'_geom_torsion_publ_flag' value 'Yes' changed to 'yes'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (6
times).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0761P)^2^] 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^)+(0.0761P)^2^]
where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3949.(5)
_cod_original_sg_symbol_H-M      P21/c
_cod_original_formula_sum        'C38 H54 N3 O9 P1'
_cod_database_code               2005644