Ligand Substitution Processes on Carbonylmetal Derivatives. 3.1Reaction of Hydridopentacarbonylchromates with Phosphines
Brunet, Jean-Jacques; Diallo, Ousmane; Donnadieu, Bruno; Roblou, Emmanuel; Organometallics 21 (2002) 3388–; doi:10.1021/om020130b

data_4076847
_publ_section_title
;
 Ligand Substitution Processes on Carbonylmetal Derivatives. 3.1Reaction
 of Hydridopentacarbonylchromates with Phosphines
;
_journal_issue                   16
_journal_name_full               Organometallics
_journal_page_first              3388
_journal_paper_doi               10.1021/om020130b
_journal_volume                  21
_journal_year                    2002
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C16 H36 Cr1 N6 O4'
_chemical_formula_structural     'C16 H36 N6 O4 CR1'
_chemical_formula_sum            'C16 H36 Cr N6 O4'
_chemical_formula_weight         490.45
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      61
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.4663(13)
_cell_length_b                   13.7007(11)
_cell_length_c                   23.544(2)
_cell_measurement_reflns_used    5630
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      20.81
_cell_measurement_theta_min      3.27
_cell_volume                     4989.0(7)
_computing_cell_refinement       'CRYSALIS-1.168(Oxford Diffraction, 2001)'
_computing_data_collection       'CRYSALIS-1.168(Oxford Diffraction, 2001)'
_computing_data_reduction        'CRYSALIS-1.168(Oxford Diffraction, 2001)'
_computing_molecular_graphics    'ORTEP-III( Burnett and Johnson,1996)'
_computing_publication_material  'WINGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1997)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Oxford-Diffraction Xcalibur'
_diffrn_measurement_method       \w
_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  0.1760
_diffrn_reflns_av_sigmaI/netI    0.0928
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            18034
_diffrn_reflns_theta_full        20.81
_diffrn_reflns_theta_max         20.81
_diffrn_reflns_theta_min         3.27
_diffrn_standards_decay_%        <0.1
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.618
_exptl_absorpt_correction_T_max  0.6826
_exptl_absorpt_correction_T_min  0.2171
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
Sheldrick, G.M. (anon) SHELX97 Release 97-2 (1998)
I/sigma threshold for reflections     =   5.000
Delta(U)/lambda**2                    =   0.000
Highest even order spherical harmonic =       8
Highest odd  order spherical harmonic =       5
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.306
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2080
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.250
_refine_diff_density_min         -0.280
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.150
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         2600
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.150
_refine_ls_R_factor_all          0.1118
_refine_ls_R_factor_gt           0.0733
_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^)+(0.0486P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1216
_refine_ls_wR_factor_ref         0.1376
_reflns_number_gt                1935
_reflns_number_total             2600
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om020130b.cif
_cod_data_source_block           er189
_cod_depositor_comments
;
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 
;
_cod_original_formula_sum        'C16 H36 Cr1 N6 O4'
_cod_database_code               4076847
_exptl_absorpt_rmerge_before     0.0945
_exptl_absorpt_rmerge_after      0.0728