Manganese 2-phosphinophosphinine precatalysts for methanol/ethanol upgrading to isobutanol.
Ward, Daniel J.; Marseglia, Margot; Saccomando, Daniel J.; Walker, Gary; Mansell, Stephen M.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 16598–16609; doi:10.1039/d4dt02142h

data_7717099
_publ_section_title
;
 Manganese 2-phosphinophosphinine precatalysts for methanol/ethanol
 upgrading to isobutanol.
;
_journal_issue                   40
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16598
_journal_page_last               16609
_journal_paper_doi               10.1039/d4dt02142h
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C25 H28 Br Mn O4 P2 Si, C6 D6'
_chemical_formula_sum            'C31 H28 Br D6 Mn O4 P2 Si'
_chemical_formula_weight         701.50
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-08-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2024-08-27 deposited with the CCDC.	2024-09-25 downloaded from the CCDC.
;
_cell_angle_alpha                69.5110(10)
_cell_angle_beta                 83.7750(10)
_cell_angle_gamma                80.4240(10)
_cell_formula_units_Z            2
_cell_length_a                   10.7367(2)
_cell_length_b                   11.6030(2)
_cell_length_c                   13.8932(3)
_cell_measurement_reflns_used    9456
_cell_measurement_temperature    101.00
_cell_measurement_theta_max      72.56
_cell_measurement_theta_min      3.40
_cell_volume                     1596.34(5)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      101.0
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0425
_diffrn_reflns_av_unetI/netI     0.0304
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            42593
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.593
_diffrn_reflns_theta_min         3.401
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.409
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.5900
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0790 before and 0.0577 after correction. The Ratio of minimum to maximum transmission is 0.7829. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_description       block
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.536
_refine_diff_density_min         -0.462
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     375
_refine_ls_number_reflns         6261
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0300
_refine_ls_R_factor_gt           0.0286
_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^)+(0.0408P)^2^+0.9439P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0758
_refine_ls_wR_factor_ref         0.0763
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6043
_reflns_number_total             6261
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02142h2.cif
_cod_data_source_block           4TMS
_cod_depositor_comments
'Adding full bibliography for 7717098--7717101.cif.'
_cod_database_code               7717099
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.740
_shelx_estimated_absorpt_t_min   0.446
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H3A,H3B,H4} of C20
 At 1.5 times of:
  {H22A,H22B,H22C} of C22, {H21A,H21B,H21C} of C21, {H19A,H19B,H19C} of C19,
  {H6A,H6B,H6C} of C6, {H20A,H20B,H20C} of C20
2.a Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C10(H10), C11(H11), C12(H12), C14(H14), C15(H15), C16(H16),
 C17(H17), C18(H18), C26(D26), C27(D27), C28(D28), C29(D29), C30(D30), C31(D31)
2.b Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,
 H21C), C22(H22A,H22B,H22C)
;
_shelx_res_checksum              43579
_shelx_hkl_checksum              84721
_olex2_submission_special_instructions 'No special instructions were received'