Stoichiometric and Catalytic Conversion of 1-Adamantyl Azide to 1-Adamantyl Isocyanate by [Cr(CO)3Cp]2and Reaction with Mo(CO)3(PiPr3)2To Form Mo(κ2-iPr3P═NN═NAd)(CO)3(PiPr3)
Fortman, George C.; Captain, Burjor; Hoff, Carl D.; Organometallics 28 (2009) 3587–; doi:10.1021/om900004k

data_4069067
_publ_section_title
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 Stoichiometric and Catalytic Conversion of 1-Adamantyl Azide to
 1-Adamantyl Isocyanate by [Cr(CO)3Cp]2and Reaction with Mo(CO)3(PiPr3)2To
 Form Mo(\k2-iPr3P&#x2550;NN&#x2550;NAd)(CO)3(PiPr3)
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_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              3587
_journal_paper_doi               10.1021/om900004k
_journal_volume                  28
_journal_year                    2009
_chemical_formula_sum            'C31 H57 Mo N3 O3 P2'
_chemical_formula_weight         677.68
_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                 95.2725(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.9113(3)
_cell_length_b                   19.1140(5)
_cell_length_c                   14.2556(3)
_cell_measurement_reflns_used    9989
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      31.12
_cell_measurement_theta_min      2.23
_cell_volume                     3503.21(14)
_computing_cell_refinement       'SAINT+  V7.46A (Bruker, 2007)'
_computing_data_collection       'APEX2 v2.2-0 (Bruker, 2007)'
_computing_data_reduction        'SAINT+  V7.46A (Bruker, 2007)'
_computing_molecular_graphics    'XSHELL v4.02 (Bruker, 2000)'
_computing_publication_material  'XCIF v6.12 (Bruker, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART APEX2 CCD diffractometer'
_diffrn_measurement_method       'omega 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  0.0240
_diffrn_reflns_av_sigmaI/netI    0.0193
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            35524
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    0.499
_exptl_absorpt_correction_T_max  0.9518
_exptl_absorpt_correction_T_min  0.8813
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS 2007/4 Bruker)'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.285
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.653
_refine_diff_density_min         -0.463
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     371
_refine_ls_number_reflns         8465
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0482
_refine_ls_R_factor_gt           0.0406
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0641P)^2^+2.9570P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1112
_refine_ls_wR_factor_ref         0.1181
_reflns_number_gt                7249
_reflns_number_total             8465
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900004k_si_002.cif
_cod_data_source_block           collect_0m
_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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
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_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4069067