Bis(triphenylphosphine)iminium Tetrachlorooxomolybdenum(V) at 150 K
Blake, A. J.; Parsons, S.; Downs, A. J.; Limberg, C.; Acta Crystallographica Section C 51 (1995) 571–573; doi:10.1107/S0108270194011303

data_2003379
_publ_section_title
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 Bis(triphenylphosphine)iminium Tetrachlorooxomolybdenum(V) at 150 K
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_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              571
_journal_page_last               573
_journal_paper_doi               10.1107/S0108270194011303
_journal_volume                  51
_journal_year                    1995
_chemical_formula_analytical
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Found: C 54.26, H 4.02, Cl 18.10, Mo 11.95, N 1.69%, Calc: C
53.95, H 4.91, Cl 17.7, Mo 11.97, N 1.75 %.
;
_chemical_formula_moiety         '[C36 H30 N P2]^+^[Cl4 Mo O]^-^'
_chemical_formula_sum            'C36 H30 Cl4 Mo N O P2'
_chemical_formula_weight         792.29
_chemical_melting_point          439.15
_chemical_name_systematic
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Bis(triphenylphosphine)iminium Tetrachloro-oxo-molybdenum(V)
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_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.470(6)
_cell_length_b                   16.765(2)
_cell_length_c                   9.6155(14)
_cell_measurement_reflns_used    44
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      16
_cell_measurement_theta_min      15
_cell_volume                     3461.0(12)
_computing_cell_refinement       'DIF4 (Stoe & Cie, 1990a)'
_computing_data_collection       'DIF4 (Stoe & Cie, 1990a)'
_computing_data_reduction        'REDU4 (Stoe & Cie, 1990b)'
_computing_molecular_graphics    'CAMERON (Pearce & Watkin, 1993)'
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution
;
SIR92 (Altomare, Cascarano, Giacovazzo & Guagliardi, 1993)
;
_diffrn_ambient_temperature      150.0(2)
_diffrn_measurement_device       'Stoe Stadi-4 four-circle'
_diffrn_measurement_method
;
\w-\q scans with on-line profile analysis (Clegg, 1981)
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_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  0.0306
_diffrn_reflns_av_sigmaI/netI    0.0425
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            3137
_diffrn_reflns_theta_max         22.52
_diffrn_reflns_theta_min         2.61
_diffrn_standards_decay_%        'not significant'
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.811
_exptl_absorpt_correction_T_max  0.621
_exptl_absorpt_correction_T_min  0.547
_exptl_absorpt_correction_type
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\y scans (North, Phillips & Mathews, 1968)
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_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.521
_exptl_crystal_description       Lath
_exptl_crystal_F_000             1604
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.487
_refine_diff_density_min         -0.607
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.06(7)
_refine_ls_extinction_coef       0.00059(13)
_refine_ls_extinction_method     SHELXL93
_refine_ls_goodness_of_fit_all   1.082
_refine_ls_goodness_of_fit_obs   1.049
_refine_ls_matrix_type           full
_refine_ls_number_parameters     407
_refine_ls_number_reflns         2739
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.088
_refine_ls_restrained_S_obs      1.049
_refine_ls_R_factor_all          0.0546
_refine_ls_R_factor_obs          0.0422
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(F~o~^2^) + 16.8557P] where P = (F~o~^2^ + 2F~c~^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0872
_refine_ls_wR_factor_obs         0.0780
_reflns_number_observed          2416
_reflns_number_total             2743
_reflns_observed_criterion       >4sigma(F)
_cod_data_source_file            mu1151.cif
_cod_data_source_block           moocl4
_cod_depositor_comments
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The following automatic conversions were performed:

'_chemical_melting_point' value '166\%' was changed to '439.15' - it
was converted from degrees Celsius(C) to
Kelvins(K).

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

'_geom_bond_publ_flag'
value 'Y' changed to 'y' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (5
times).

'_geom_angle_publ_flag' value 'Y' changed to 'y' according
to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29 (10 times).

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^(F~o~^2^) +
16.8557P] where P = (F~o~^2^ + 2F~c~^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^(F~o~^2^) + 16.8557P] where P =
(F~o~^2^ + 2F~c~^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_database_code               2003379