Reaction of N-methyldihydropyridines with alkoxycarbene complexes of chromium and tungsten: sequential use of three carbonyl ligands of Cr(CO)6 for the formation of polyoxygenated compounds
Rudler, Henri; Parlier, Andrée; Martin-Vaca, Blanca; Garrier, Eva; Vaissermann, Jacqueline; Chemical Communications  (1999) 1439–; doi:10.1039/a903474i

data_7110582
_publ_section_title
;
 Reaction of N-methyldihydropyridines with alkoxycarbene complexes of
 chromium and tungsten: sequential use of three carbonyl ligands of
 Cr(CO)6 for the formation of polyoxygenated compounds
;
_journal_issue                   15
_journal_name_full               'Chemical Communications'
_journal_page_first              1439
_journal_paper_doi               10.1039/a903474i
_journal_year                    1999
_chemical_compound_source
;
?
;
_chemical_formula_moiety         ' C23 H24 O3 '
_chemical_formula_sum            'C23 H24 O3'
_chemical_formula_weight         348.44
_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P -2yc'
_symmetry_space_group_name_H-M   'P 1 c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 90.26(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.198(5)
_cell_length_b                   6.867(1)
_cell_length_c                   12.192(18)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298
_cell_measurement_theta_max      13.5
_cell_measurement_theta_min      13
_cell_volume                     937.5(15)
_diffrn_ambient_temperature      295
_diffrn_measurement_device       '  Enraf-nonius CAD4 '
_diffrn_measurement_method       2\q/\w
_diffrn_radiation_monochromator  ' graphite'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.04
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            3075
_diffrn_reflns_theta_max         30
_diffrn_reflns_theta_min         1
_diffrn_standards_decay_%        none
_diffrn_standards_interval_time  3600s
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.08
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            ' colourless '
_exptl_crystal_density_diffrn    1.23
_exptl_crystal_description       ' plate '
_exptl_crystal_F_000             372.10
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.29
_refine_diff_density_min         -0.24
_refine_ls_extinction_coef       53.4
_refine_ls_extinction_method     'Larson 1970 Crystallographic Computing eq 22'
_refine_ls_goodness_of_fit_obs   1.0758
_refine_ls_hydrogen_treatment
;
 one overall isotropic thermal parameter refined
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     237
_refine_ls_number_reflns         1806
_refine_ls_R_factor_obs          0.0511
_refine_ls_shift/esd_max         0.087555
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme
;
 Chebychev polynomial (Carruthers & Watkin, 1979)
;
_refine_ls_wR_factor_obs         0.0643
_reflns_limit_h_max              15
_reflns_limit_h_min              -15
_reflns_limit_k_max              9
_reflns_limit_k_min              0
_reflns_limit_l_max              17
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_reflns_number_observed          1806
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_reflns_observed_criterion       >3.00\s(I)
_cod_data_source_file            903474isup1.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_cell_measurement_temperature' value '298K' was changed to '298' -
the value should be numeric and without a unit
designator.

'_diffrn_ambient_temperature' value '295K' was changed
to '295' - the value should be numeric and without a unit
designator.

'_symmetry_cell_setting' value 'Monoclinic ' changed to
'monoclinic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from
2011-04-26.

'_refine_ls_matrix_type' value ' full ' changed to
'full' 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 

The following automatic conversions were performed:

'_atom_sites_solution_primary' value ' Direct_Methods ' was changed
to 'direct'.

'_atom_sites_solution_hydrogens' value ' Difference Fourier map ' was
changed to 'difmap'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_cell_volume        937(1)
_cod_original_sg_symbol_H-M      'P 1 c 1 '
_cod_original_formula_sum        ' C23 H24 O3 '
_cod_database_code               7110582