2H-1-Benzopyrans. 4-Chloro-3-methoxycarbonyl-2-dimethoxyphosphoryl-2H-1-benzopyran, (I) and 4-Chloro-2-dimethoxyphosphoryl-2H-1-benzopyran, (II)
Olszak, Tomasz A.; Grabowski, Mieczysław J.; Stępień, Andrzej; Modranka, R.; Kostka, K.; Acta Crystallographica Section C 53 (1997) 1514–1516; doi:10.1107/S010827019700735X

data_2006606
_publ_section_title
;
2H-1-Benzopyrans.
4-Chloro-3-methoxycarbonyl-2-dimethoxyphosphoryl-2H-1-benzopyran, (I)
and 4-Chloro-2-dimethoxyphosphoryl-2H-1-benzopyran, (II)
;
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1514
_journal_page_last               1516
_journal_paper_doi               10.1107/S010827019700735X
_journal_volume                  53
_journal_year                    1997
_chemical_formula_analytical     'C11 H12 Cl1 O4 P1 '
_chemical_formula_moiety         'C11 H12 Cl1 O4 P1 '
_chemical_formula_structural     'C11 H12 Cl1 O4 P1 '
_chemical_formula_sum            'C11 H12 Cl O4 P'
_chemical_formula_weight         274.64
_chemical_melting_point          330(2)
_chemical_name_systematic
;
4-chloro-2-dimethoxyphosphoryl-2H-1-benzopyran
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                108.444(7)
_cell_angle_beta                 92.736(7)
_cell_angle_gamma                82.800(7)
_cell_formula_units_Z            2
_cell_length_a                   7.8864(5)
_cell_length_b                   11.3138(10)
_cell_length_c                   7.2675(6)
_cell_measurement_reflns_used    23
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      34.09
_cell_measurement_theta_min      22.72
_cell_volume                     610.26(9)
_computing_cell_refinement       'MSC/AFC Diffractometer Control Software'
_computing_data_collection
;MSC/AFC Diffractometer Control Software (Molecular Structure Corporation,
 1988)
;
_computing_data_reduction
'TEXSAN (Molecular Structure Corporation, 1989)'
_computing_molecular_graphics    'ORTEX  (McArdle, 1995)'
_computing_publication_material  'PARST (Nardelli, 1993)'
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'AFC5S Rigaku Diffractometer'
_diffrn_measurement_method       '\w scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0136
_diffrn_reflns_av_sigmaI/netI    0.0366
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            1915
_diffrn_reflns_theta_max         60.07
_diffrn_reflns_theta_min         4.15
_diffrn_standards_decay_%        <2
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.0410
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.898
_exptl_absorpt_correction_type
'empirical \y scan (North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.4946
_exptl_crystal_description       prism
_exptl_crystal_F_000             284
_exptl_crystal_size_max          .2
_exptl_crystal_size_mid          .1
_exptl_crystal_size_min          .1
_refine_diff_density_max         0.252
_refine_diff_density_min         -0.186
_refine_ls_extinction_coef       0.0140(12)
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   0.966
_refine_ls_goodness_of_fit_obs   1.082
_refine_ls_hydrogen_treatment
;
Methoxy H atoms refined as rigid body with fixed displacement parameters,
other H atoms refined isotropically
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     185
_refine_ls_number_reflns         1791
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.966
_refine_ls_restrained_S_obs      1.082
_refine_ls_R_factor_all          0.0469
_refine_ls_R_factor_obs          .0325
_refine_ls_shift/esd_max         0.008
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0571P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0910
_refine_ls_wR_factor_obs         .0881
_reflns_number_observed          1384
_reflns_number_total             1791
_reflns_observed_criterion       >2\s(I)
_cod_data_source_file            na1207.cif
_cod_data_source_block           II
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0571P)^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^)+(0.0571P)^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        610.26(8)
_cod_original_formula_sum        'C11 H12 Cl1 O4 P1 '
_cod_database_code               2006606