Phosphino and Phosphonito Carbyne Complexes: [Mo(\τb CX)(CO)2{HB(pzMe2)3}] (X = PPh2, P(═O)(OEt)2; pz = Pyrazol-1-yl)
Cordiner, Richard L.; Gugger, Paul A.; Hill, Anthony F.; Willis, Anthony C.; Organometallics 28 (2009) 6632–; doi:10.1021/om900868s

data_4070494
_publ_section_title
;
 Phosphino and Phosphonito Carbyne Complexes: [Mo(\\tb
 CX)(CO)2{HB(pzMe2)3}] (X = PPh2, P(&#x2550;O)(OEt)2; pz = Pyrazol-1-yl)
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              6632
_journal_paper_doi               10.1021/om900868s
_journal_volume                  28
_journal_year                    2009
_chemical_compound_source        local
_chemical_formula_moiety         'C30 H32 B Mo N6 O2 P '
_chemical_formula_sum            'C30 H32 B Mo N6 O2 P'
_chemical_formula_weight         646.35
_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
_audit_creation_date             08-03-20
_audit_creation_method           CRYSTALS_ver_12.18
_audit_update_record
;
2008-03-25 - Report on C30 H32 B Mo N6 O2 P 
            by Anthony C. Willis
            for Anthony F. Hill, Richard Cordiner

2008-03-25 - passes checkcif tests with minor warnings

;
_cell_angle_alpha                76.1021(8)
_cell_angle_beta                 87.0370(12)
_cell_angle_gamma                81.2670(11)
_cell_formula_units_Z            2
_cell_length_a                   8.1834(1)
_cell_length_b                   10.1992(2)
_cell_length_c                   18.8867(4)
_cell_measurement_reflns_used    25208
_cell_measurement_temperature    200
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.7
_cell_volume                     1512.28(5)
_computing_cell_refinement       'Denzo/Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius BV, 1997)'
_computing_data_reduction        'Denzo/Scalepack (Otwinowski & Minor, 1997)'
_computing_molecular_graphics
; 
ORTEP-II (Johnson 1976) in teXsan (MSC, 1992-1997)
;
_computing_publication_material  'CRYSTALS (Watkin et al 2003)'
_computing_structure_refinement  'CRYSTALS (Watkin et al 2003)'
_computing_structure_solution    'SIR92 (Altomare et al, 1994)'
_diffrn_ambient_temperature      200
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       ' \f and \w scans with CCD '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.035
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            31171
_diffrn_reflns_theta_full        27.477
_diffrn_reflns_theta_max         27.477
_diffrn_reflns_theta_min         2.577
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.524
_exptl_absorpt_correction_T_max  0.972
_exptl_absorpt_correction_T_min  0.883
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
via Gaussian method (Coppens, 1970) implemented in maXus (Mackay et al, 2000)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_density_meas      ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.40
_refine_diff_density_min         -0.61
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9754
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         6917
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0364
_refine_ls_R_factor_gt           0.0305
_refine_ls_shift/su_max          0.002614
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.04P)^2^ + 0.46P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0836
_refine_ls_wR_factor_gt          0.0815
_refine_ls_wR_factor_ref         0.0836
_reflns_limit_h_max              10
_reflns_limit_h_min              -10
_reflns_limit_k_max              13
_reflns_limit_k_min              -12
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                6060
_reflns_number_total             6917
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.39
_oxford_diffrn_Wilson_scale      2.13
_oxford_refine_ls_scale          0.7448(12)
_oxford_structure_analysis_title '3201523 hil0801'
_cod_data_source_file            om900868s_si_001.cif
_cod_data_source_block           hil0801
_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.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

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_sg_symbol_H-M      'P -1 '
_cod_database_code               4070494