Isolation and structural determination of two derivatives of the elusive carbamic acid
Aresta, Michele; Ballivet-Tkatchenko, Danielle; Dell’Amico, Daniela Belli; Boschi, Daniele; Calderazzo, Fausto; Labella, Luca; Bonnet, Michel C.; Faure, René; Marchetti, Fabio; Chemical Communications  (2000) 1099–; doi:10.1039/b002479l

data_7110952
_publ_section_title
;
 Isolation and structural determination of two derivatives of the elusive
 carbamic acid
;
_journal_issue                   13
_journal_name_full               'Chemical Communications'
_journal_page_first              1099
_journal_paper_doi               10.1039/b002479l
_journal_year                    2000
_chemical_formula_sum            'C17 H26 Cl Co N3 O8 P'
_chemical_formula_weight         525.76
_chemical_name_systematic
; 
N-carboxy-P-phenyl-P-dinitrosylchlorocobalt(i)-1-aza-4,6-dioxa-5-
phosphacycl
oottane 
;
_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                73.34(2)
_cell_angle_beta                 69.94(2)
_cell_angle_gamma                66.18(2)
_cell_formula_units_Z            2
_cell_length_a                   9.612(2)
_cell_length_b                   11.936(3)
_cell_length_c                   12.371(4)
_cell_measurement_temperature    293(2)
_cell_volume                     1201.4(6)
_computing_cell_refinement       'SDP package'
_computing_data_collection       'SDP package'
_computing_data_reduction        'SDP package'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.560
_diffrn_measured_fraction_theta_max 0.560
_diffrn_measurement_device_type  'Nonius CAD-4'
_diffrn_measurement_method       '2\q/\w scans'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0127
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3918
_diffrn_reflns_theta_full        29.97
_diffrn_reflns_theta_max         29.97
_diffrn_reflns_theta_min         1.89
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.937
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'Dark brown'
_exptl_crystal_density_diffrn    1.453
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             544
_exptl_crystal_size_max          '0.40 mm'
_exptl_crystal_size_mid          '0.25 mm'
_exptl_crystal_size_min          '0.25 mm'
_refine_diff_density_max         0.944
_refine_diff_density_min         -1.446
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.157
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         3918
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.157
_refine_ls_R_factor_all          0.1321
_refine_ls_R_factor_gt           0.0915
_refine_ls_shift/su_max          0.030
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1851P)^2^+2.7509P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2348
_refine_ls_wR_factor_ref         0.3093
_reflns_number_gt                2977
_reflns_number_total             3918
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b002479lsup1.cif
_cod_data_source_block           fau
_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 2.4.2 from
2011-04-26.

'_exptl_absorpt_correction_type' value 'Empirical'
changed to 'empirical' 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 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7110952