Small-Molecule Activation within the Group 6 Complexes (η5-C5Me5)[N(iPr)C(Me)N(iPr)]M(CO)(L) for M = Mo, W and L = N2, NCMe, η2-Alkene, SMe2, C3H6O
Farrell, Wesley S.; Yonke, Brendan L.; Reeds, Jonathan P.; Zavalij, Peter Y.; Sita, Lawrence R.; Organometallics 35 (2016) 1132–; doi:10.1021/acs.organomet.6b00131

data_4086466
_publ_section_title
;
 Small-Molecule Activation within the Group 6 Complexes
 (\h5-C5Me5)[N(iPr)C(Me)N(iPr)]M(CO)(L) for M = Mo, W and L = N2, NCMe,
 \h2-Alkene, SMe2, C3H6O
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              1132
_journal_paper_doi               10.1021/acs.organomet.6b00131
_journal_volume                  35
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C21 H38 N2 O S W'
_chemical_formula_sum            'C21 H38 N2 O S W'
_chemical_formula_weight         550.44
_chemical_name_common            W-complex
_chemical_name_systematic
;
W-complex
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL-2014 & ZCIF'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.7355(4)
_cell_length_b                   15.6039(6)
_cell_length_c                   16.2732(7)
_cell_measurement_reflns_used    15862
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.7
_cell_measurement_theta_min      2.5
_cell_volume                     2218.17(16)
_computing_cell_refinement       Apex2
_computing_data_collection       'Apex2 (Bruker, 2010)'
_computing_data_reduction        'Apex2, Saint'
_computing_molecular_graphics    'XSHEL (Bruker, 2004)'
_computing_publication_material  'Apex2, SHELXL-2014, Platon (Spek, 1990)'
_computing_structure_refinement  'ShelXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'ShelXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Smart Apex II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_measurement_specimen_support 'MiTeGen loop'
_diffrn_orient_matrix_type       standard
_diffrn_orient_matrix_UB_11      -0.0423432
_diffrn_orient_matrix_UB_12      0.0501211
_diffrn_orient_matrix_UB_13      -0.0308252
_diffrn_orient_matrix_UB_21      -0.0308354
_diffrn_orient_matrix_UB_22      -0.0388920
_diffrn_orient_matrix_UB_23      -0.0459502
_diffrn_orient_matrix_UB_31      -0.1017871
_diffrn_orient_matrix_UB_32      -0.0090804
_diffrn_orient_matrix_UB_33      0.0267308
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0209
_diffrn_reflns_av_unetI/netI     0.0165
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            29685
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        26.500
_diffrn_reflns_theta_max         29.999
_diffrn_reflns_theta_min         1.808
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    5.314
_exptl_absorpt_correction_T_max  0.279
_exptl_absorpt_correction_T_min  0.195
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.648
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.849
_refine_diff_density_min         -0.583
_refine_diff_density_rms         0.077
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.482(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         6418
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0178
_refine_ls_R_factor_gt           0.0156
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0100P)^2^+1.5200P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0315
_refine_ls_wR_factor_ref         0.0322
_reflns_Friedel_coverage         0.771
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                6017
_reflns_number_total             6418
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00131_si_001.cif
_cod_data_source_block           cmpd_16
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 4086460--4086471.cif.
;
_cod_original_sg_symbol_H-M      P212121
_cod_database_code               4086466
_shelx_estimated_absorpt_t_min   0.258
_shelx_estimated_absorpt_t_max   0.362
_shelxl_version_number           2014-3
_shelx_res_checksum              24652
_shelx_hkl_checksum              32296