Ultrafast Photochemistry of a Molybdenum Carbonyl-Nitrosyl Complex with a Triazacyclononane Coligand
Gessner, Niklas; Bäck, Anna Karina; Knorr, Johannes; Nagel, Christoph; Marquetand, Philipp; Schatzschneider, Ulrich; González, Leticia; Nuernberger, Patrick; Physical Chemistry Chemical Physics  (2021) –; doi:10.1039/D1CP03514B

data_7243527
_publ_section_title
;
 Ultrafast Photochemistry of a Molybdenum Carbonyl-Nitrosyl Complex with a
 Triazacyclononane Coligand
;
_journal_name_full               'Physical Chemistry Chemical Physics'
_journal_paper_doi               10.1039/D1CP03514B
_journal_year                    2021
_chemical_formula_moiety         'C17 H33 Mo N4 O3, F6 P'
_chemical_formula_sum            'C17 H33 F6 Mo N4 O3 P'
_chemical_formula_weight         582.37
_chemical_name_systematic        '[Mo(CO)2(NO)(iPr3tacn)]PF6'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_Int_Tables_number      61
_audit_creation_date             2015-08-05
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-08-05 deposited with the CCDC.	2021-09-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.1434(16)
_cell_length_b                   14.9459(14)
_cell_length_c                   18.1606(17)
_cell_measurement_temperature    100.00
_cell_volume                     4653.2(8)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.00
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.9985
_diffrn_measured_fraction_theta_max 0.9985
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0554
_diffrn_reflns_av_unetI/netI     0.0266
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            68440
_diffrn_reflns_theta_full        25.9977
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.13
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.707
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6825
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0613 before and 0.0574 after correction.
The Ratio of minimum to maximum transmission is 0.9152.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.6625
_exptl_crystal_description       block
_exptl_crystal_F_000             2372.4946
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.384
_exptl_crystal_size_min          0.248
_refine_diff_density_max         0.4816
_refine_diff_density_min         -0.3588
_refine_diff_density_rms         0.0855
_refine_ls_d_res_high            0.8107
_refine_ls_d_res_low             9.5733
_refine_ls_goodness_of_fit_ref   1.0102
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    53
_refine_ls_number_parameters     295
_refine_ls_number_reflns         4562
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0102
_refine_ls_R_factor_all          0.0304
_refine_ls_R_factor_gt           0.0223
_refine_ls_shift/su_max          0.0001
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0148P)^2^+6.6870P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0469
_refine_ls_wR_factor_ref         0.0536
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              21
_reflns_limit_h_min              0
_reflns_limit_k_max              18
_reflns_limit_k_min              0
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                3891
_reflns_number_total             4562
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d1cp03514b2.cif
_cod_data_source_block           CN14015
_cod_database_code               7243527
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{N1b, C2a}
{C2b, N1a}
3. Uiso/Uaniso restraints and constraints
Uanis(C2b) = Uanis(N1a)
Uanis(N1b) = Uanis(C2a)
4. Others
 Sof(C2a)=Sof(N1a)=1-FVAR(1)
 Sof(C2b)=Sof(N1b)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C10(H10), C13(H13), C16(H16)
5.b Secondary CH2 refined with riding coordinates:
 C3(H3a,H3b), C4(H4a,H4b), C5(H5a,H5b), C6(H6a,H6b), C7(H7a,H7b), C8(H8a,H8b)
5.c Idealised Me refined as rotating group:
 C9(H9a,H9b,H9c), C11(H11a,H11b,H11c), C12(H12a,H12b,H12c), C14(H14a,H14b,
 H14c), C15(H15a,H15b,H15c), C17(H17a,H17b,H17c)
;
_olex2_date_sample_data_collection 2014-02-05
_olex2_date_sample_submission    2014-02-05
_olex2_exptl_crystal_mounting_method
'crystal was mounted with perfluorated polyether oil'
_olex2_submission_original_sample_id 'USC CN 071 '
_olex2_submission_special_instructions 'No special instructions were received'