Tungsten and molybdenum dinitrogen complexes supported by a pentadentate tetrapodal phosphine ligand: comparative spectroscopic, electrochemical and reactivity studies.
Junge, Jannik; Froitzheim, Sven; Engesser, Tobias A.; Krahmer, Jan; Näther, Christian; Le Poul, Nicolas; Tuczek, Felix; Dalton transactions (Cambridge, England : 2003) 51 (2022) 6166–6176; doi:10.1039/d1dt04212b

data_7710098
_publ_section_title
;
 Tungsten and molybdenum dinitrogen complexes supported by a pentadentate
 tetrapodal phosphine ligand: comparative spectroscopic, electrochemical
 and reactivity studies.
;
_journal_issue                   16
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6166
_journal_page_last               6176
_journal_paper_doi               10.1039/d1dt04212b
_journal_volume                  51
_journal_year                    2022
_chemical_formula_sum            'C39 H53 N2 P5 W'
_chemical_formula_weight         888.53
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-12-10 deposited with the CCDC.	2022-03-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.168(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.2033(8)
_cell_length_b                   9.4433(3)
_cell_length_c                   21.9208(10)
_cell_measurement_reflns_used    59003
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.003
_cell_measurement_theta_min      1.678
_cell_volume                     3798.1(3)
_computing_cell_refinement       'X-AREA (STOE, 2008)'
_computing_data_collection       'X-AREA (STOE, 2008)'
_computing_data_reduction        'X-AREA (STOE, 2008)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'STOE IPDS-2'
_diffrn_measurement_method       'Omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0542
_diffrn_reflns_av_unetI/netI     0.0235
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            59003
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.003
_diffrn_reflns_theta_min         1.678
_exptl_absorpt_coefficient_mu    3.283
_exptl_absorpt_correction_T_max  0.6463
_exptl_absorpt_correction_T_min  0.3161
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-Red and X-Shape (STOE, 2008)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.554
_exptl_crystal_description       block
_exptl_crystal_F_000             1800
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.096
_refine_diff_density_min         -1.154
_refine_diff_density_rms         0.110
_refine_ls_extinction_coef       0.00220(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     430
_refine_ls_number_reflns         9164
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0402
_refine_ls_R_factor_gt           0.0365
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0521P)^2^+4.8765P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0899
_refine_ls_wR_factor_ref         0.0921
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8455
_reflns_number_total             9164
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt04212b2.cif
_cod_data_source_block           felix193
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7710098
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              6855
_shelx_hkl_checksum              835