Synthesis and Characterization of Hydrido Carbonyl Molybdenum and Tungsten PNP Pincer Complexes.
Oztopcu, Ozgür; Holzhacker, Christian; Puchberger, Michael; Weil, Matthias; Mereiter, Kurt; Veiros, Luis F.; Kirchner, Karl; Organometallics 32 (2013) 3042–3052; doi:10.1021/om400254k

data_4080847
_publ_section_title
;
 Synthesis and Characterization of Hydrido Carbonyl Molybdenum and
 Tungsten PNP Pincer Complexes.
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              3042
_journal_page_last               3052
_journal_paper_doi               10.1021/om400254k
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C32 H25 Br N3 O4 P2 W, Br, C H4 O'
_chemical_formula_sum            'C33 H29 Br2 N3 O4 P2 W'
_chemical_formula_weight         937.20
_chemical_name_common            '1648 [W(PNP-Ph)(CO)3Br]Br.CH3OH (3a.CH3OH)'
_chemical_name_systematic
; 
[W(PNP-Ph)(CO)3Br]Br.CH3OH (3a.CH3OH)
;
_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                99.456(3)
_cell_angle_beta                 95.412(3)
_cell_angle_gamma                104.306(3)
_cell_formula_units_Z            2
_cell_length_a                   10.1741(6)
_cell_length_b                   13.1580(7)
_cell_length_c                   14.1040(8)
_cell_measurement_reflns_used    9892
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      2.28
_cell_volume                     1786.64(18)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT, SADABS, XPREP'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \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  0.0598
_diffrn_reflns_av_sigmaI/netI    0.0563
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            46633
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         1.98
_exptl_absorpt_coefficient_mu    5.598
_exptl_absorpt_correction_T_max  0.77
_exptl_absorpt_correction_T_min  0.56
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'program SADABS'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.742
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             908
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
Crystals were grown from methanol at -20 deg Celsius.
The compound contains in addition to a free bromide 
ion Br2, which is N-H...Br hydrogen bonded to N2, 
disordered methanol with an obvious oxygen position at ca.
2.8 A distance from N3. This disordered solvent was squeezed 
with program PLATON. The solvent is in an infinite channel
along the a-axis, which houses also the free Br anions.
Chemical formula and quantities derived thereof 
are given for the formula WBr(CO)3(PNP-ph).Br.CH3OH.
;
_refine_diff_density_max         1.56
_refine_diff_density_min         -1.39
_refine_diff_density_rms         0.12
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.980
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         10395
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.982
_refine_ls_R_factor_all          0.0625
_refine_ls_R_factor_gt           0.0385
_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^)+(0.0438P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0822
_refine_ls_wR_factor_ref         0.0884
_reflns_number_gt                7880
_reflns_number_total             10395
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400254k_si_001.cif
_cod_data_source_block           3a-1648
_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 2.3.1 from 2005-06-27.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        1786.63(17)
_cod_original_sg_symbol_Hall     '-P 1   '
_cod_original_sg_symbol_H-M      'P -1   '
_cod_database_code               4080847