The pyrrole ring η(2)-hapticity bridged binuclear tricarbonyl Mo(0) and W(0) complexes: catalysis of regioselective hydroamination reactions and DFT calculations.
Jha, Vikesh Kumar; Mani, Ganesan; Davuluri, Yogeswara Rao; Anoop, Anakuthil; Dalton transactions (Cambridge, England : 2003) 46 (2017) 1840–1847; doi:10.1039/c6dt04458a

data_7041647
_publ_section_title
;
 The pyrrole ring \h(2)-hapticity bridged binuclear tricarbonyl Mo(0) and
 W(0) complexes: catalysis of regioselective hydroamination reactions and
 DFT calculations.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1840
_journal_page_last               1847
_journal_paper_doi               10.1039/c6dt04458a
_journal_volume                  46
_journal_year                    2017
_chemical_formula_sum            'C40 H49 N9 O7.5 W2'
_chemical_formula_weight         1143.58
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-01-02 deposited with the CCDC.
2017-01-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.005(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.4325(9)
_cell_length_b                   14.7737(9)
_cell_length_c                   20.2936(13)
_cell_measurement_reflns_used    25049
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.999
_cell_measurement_theta_min      1.985
_cell_volume                     4273.7(5)
_computing_data_collection       'SMART APEX'
_computing_molecular_graphics    ortep
_computing_publication_material  WinGx
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    sir92
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Brucker CCD APEX 2'
_diffrn_measurement_method       hemisphere
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0310
_diffrn_reflns_av_unetI/netI     0.0191
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            25049
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.985
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    5.439
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.777
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2240
_exptl_crystal_size_max          0.188
_exptl_crystal_size_mid          0.177
_exptl_crystal_size_min          0.114
_exptl_transmission_factor_max   1.00
_exptl_transmission_factor_min   0.63
_platon_squeeze_details
;
The SQUEEZE/PLATON procedure yielded total void volume and electron 
count of 620\%A^3^ and 58 e, respectively. For Z = 4 this gives
14.5 electrons per formula. This number equals about one half of THF molecule
per fromula or 1.45 THF molecules per unit cell.
The fraction of solvent has been treated as a diffuse contribution 
to the overall scattering without specific atom positions.

 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_refine_diff_density_max         1.091
_refine_diff_density_min         -1.054
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     259
_refine_ls_number_reflns         3773
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0229
_refine_ls_R_factor_gt           0.0209
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0277P)^2^+12.7564P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0514
_refine_ls_wR_factor_ref         0.0524
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3531
_reflns_number_total             3773
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04458a2.cif
_cod_data_source_block           W
_cod_depositor_comments
'Adding full bibliography for 7041646--7041647.cif.'
_cod_original_formula_sum        'C40 H49 N9 O7.50 W2'
_cod_database_code               7041647
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.428
_shelx_estimated_absorpt_t_max   0.576
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              43887
_shelx_fab_checksum              51374