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_7717100
_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'
_chemical_formula_sum            'C24 H26 Br Mn O4 P2 Si'
_chemical_formula_weight         603.33
_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     iterative
_audit_creation_date             2022-06-14
_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                73.526(6)
_cell_angle_beta                 73.880(6)
_cell_angle_gamma                87.503(7)
_cell_formula_units_Z            2
_cell_length_a                   9.1873(8)
_cell_length_b                   11.3280(11)
_cell_length_c                   13.6859(11)
_cell_measurement_reflns_used    2693
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      63.28
_cell_measurement_theta_min      3.50
_cell_volume                     1311.2(2)
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device       'three-circle diffractometer'
_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_unetI/netI     0.0792
_diffrn_reflns_Laue_measured_fraction_full 0.962
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4238
_diffrn_reflns_point_group_measured_fraction_full 0.962
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        64.300
_diffrn_reflns_theta_max         64.300
_diffrn_reflns_theta_min         3.505
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.706
_exptl_absorpt_correction_T_max  0.7524
_exptl_absorpt_correction_T_min  0.3909
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.

Final HKLF 4 output contains 32339 reflections, Rint = 0.1083
 (12207 with I > 3sig(I), Rint = 0.0770)
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.528
_exptl_crystal_description       plate
_exptl_crystal_F_000             612
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.212
_refine_diff_density_min         -1.129
_refine_diff_density_rms         0.206
_refine_ls_extinction_coef       0.0033(7)
_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   1.077
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         4238
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.1157
_refine_ls_R_factor_gt           0.0900
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1167P)^2^+13.5469P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2217
_refine_ls_wR_factor_ref         0.2492
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3331
_reflns_number_total             4238
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02142h2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7717098--7717101.cif.'
_cod_database_code               7717100
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.861
_shelx_estimated_absorpt_t_min   0.372
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.551(3)
 0.449(3)
2. 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
3. Restrained distances
 H1-O1
 1 with sigma of 0.05
4.a Ternary CH refined with riding coordinates:
 C1(H1A)
4.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)
4.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C)
;
_shelx_res_checksum              71457
_shelx_hkl_checksum              92468
_olex2_submission_special_instructions 'No special instructions were received'