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_7717101
_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         'C24 H26 Br Mn O4 P2 Si, C H4 O'
_chemical_formula_sum            'C25 H30 Br Mn O5 P2 Si'
_chemical_formula_weight         635.37
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2024-04-22
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2024-08-20 deposited with the CCDC.	2024-09-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.7740(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.2627(3)
_cell_length_b                   13.7362(3)
_cell_length_c                   14.3867(3)
_cell_measurement_reflns_used    9708
_cell_measurement_temperature    107(2)
_cell_measurement_theta_max      72.068
_cell_measurement_theta_min      4.160
_cell_volume                     2804.27(10)
_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      107.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_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  0.0393
_diffrn_reflns_av_unetI/netI     0.0203
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            55731
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.225
_diffrn_reflns_theta_min         4.160
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.263
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.5164
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1358 before and 0.0613 after correction. The Ratio of minimum to maximum transmission is 0.6852. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.505
_exptl_crystal_description       block
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.421
_refine_diff_density_min         -0.520
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         5514
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0280
_refine_ls_R_factor_gt           0.0268
_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^)+(0.0312P)^2^+3.1616P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0677
_refine_ls_wR_factor_ref         0.0685
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5304
_reflns_number_total             5514
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02142h2.cif
_cod_data_source_block           3_MeOH
_cod_depositor_comments
'Adding full bibliography for 7717098--7717101.cif.'
_cod_database_code               7717101
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.476
_shelx_estimated_absorpt_t_min   0.180
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups, All O(H) groups
2. Restrained distances
 O5-C25 \\sim O6-C25
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O5) = Uanis(O6)
4. Others
 Sof(O6)=Sof(H6)=Sof(H25D)=Sof(H25E)=Sof(H25F)=1-FVAR(1)
 Sof(O5)=Sof(H5)=Sof(H25A)=Sof(H25B)=Sof(H25C)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C1(H1A)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12), C14(H14),
 C15(H15), C16(H16), C17(H17), C18(H18)
5.c Tetrahedral OH refined with riding coordinates:
 O5(H5), O6(H6)
5.d Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,
 H21C), C25(H25A,H25B,H25C), C25(H25D,H25E,H25F)
5.e Idealised tetrahedral OH refined as rotating group:
 O1(H1)
;
_shelx_res_checksum              11470
_shelx_hkl_checksum              54861
_olex2_submission_special_instructions 'No special instructions were received'