Efficient hydrogenation of ketones over the diaminophosphino manganese complex.
Zhang, Yu; Li, Bin; Wang, Tao; Duan, Ning; Zheng, Jianwei; Li, Hao; Zhang, Fengjun; Fang, Xiaolong; Dalton transactions (Cambridge, England : 2003) 53 (2024) 16475–16479; doi:10.1039/d4dt02297a

data_7717031
_publ_section_title
;
 Efficient hydrogenation of ketones over the diaminophosphino manganese
 complex.
;
_journal_issue                   40
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16475
_journal_page_last               16479
_journal_paper_doi               10.1039/d4dt02297a
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'Br, C42 H38 Mn N2 O2 P2'
_chemical_formula_sum            'C42 H38 Br Mn N2 O2 P2'
_chemical_formula_weight         799.53
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-07-19
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2024-08-06 deposited with the CCDC.	2024-09-16 downloaded from the CCDC.
;
_cell_angle_alpha                92.962(11)
_cell_angle_beta                 105.097(13)
_cell_angle_gamma                90.746(13)
_cell_formula_units_Z            4
_cell_length_a                   11.757(2)
_cell_length_b                   17.831(3)
_cell_length_c                   18.477(3)
_cell_measurement_reflns_used    13468
_cell_measurement_temperature    150
_cell_measurement_theta_max      69.60
_cell_measurement_theta_min      3.90
_cell_volume                     3733.4(11)
_computing_cell_refinement       'X-Area Recipe 1.33.0.0 (STOE, 2015)'
_computing_data_collection       'X-Area Pilatus3_SV 1.31.153.0 (STOE, 2018)'
_computing_data_reduction
;
X-Area Integrate 1.74.2.0 (STOE, 2018)
X-Area LANA 1.75.3.0 (STOE, 2018)
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150
_diffrn_detector                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 300K'
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details      '1369 frames, detector distance = 40 mm'
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '1.2 mm, 0.6 diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  270
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0812
_diffrn_reflns_av_unetI/netI     0.1019
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            28733
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        62.500
_diffrn_reflns_theta_max         62.500
_diffrn_reflns_theta_min         3.609
_diffrn_source                   'GeniX 3D HF Cu'
_diffrn_source_current           0.600
_diffrn_source_power             0.030
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    5.241
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.2669
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.422
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1640
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.444
_refine_diff_density_min         -0.797
_refine_diff_density_rms         0.222
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     901
_refine_ls_number_reflns         11783
_refine_ls_number_restraints     972
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.1294
_refine_ls_R_factor_gt           0.0756
_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^)+(0.1662P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1906
_refine_ls_wR_factor_ref         0.2572
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7500
_reflns_number_total             11783
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02297a2.cif
_cod_data_source_block           20240113-3
_cod_depositor_comments          'Adding full bibliography for 7717031.cif.'
_cod_original_cell_volume        3733.4(10)
_cod_database_code               7717031
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2. Uiso/Uaniso restraints and constraints
C00H \\sim C00I \\sim C1 \\sim C00K \\sim C00L \\sim C00M \\sim C00N \\sim C00O
\\sim C4 \\sim C00Q \\sim C00R \\sim C00S \\sim C00T \\sim C00U \\sim C00V
\\sim C00W \\sim C00X \\sim C00Y \\sim C00Z \\sim C010 \\sim C011 \\sim C3
\\sim C013 \\sim C014 \\sim C015 \\sim C016 \\sim C017 \\sim C018 \\sim C019
\\sim C01A \\sim C01B \\sim C01C \\sim C01D \\sim C01E \\sim C2 \\sim C01G
\\sim C01H \\sim C01I \\sim C01J \\sim C01K \\sim C01L \\sim C01M \\sim C01N
\\sim C01O \\sim C01P \\sim C01Q \\sim C01R \\sim C01S \\sim C01T \\sim C01U
\\sim C01V \\sim C01W \\sim C01X \\sim C01Y \\sim C01Z \\sim C020 \\sim C021
\\sim C022 \\sim C023 \\sim C024 \\sim C025 \\sim C026 \\sim C027 \\sim C028
\\sim C029 \\sim C02A \\sim C02B \\sim C02C \\sim C02D \\sim C02E \\sim C02F
\\sim C02G \\sim C02H \\sim C02I \\sim C02J \\sim C02K \\sim C02L \\sim C02M
\\sim C02N \\sim C02O \\sim C02P \\sim C02Q \\sim C02R \\sim C02S: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(C00H) \\sim Ueq, Uanis(C00I) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C00K)
\\sim Ueq, Uanis(C00L) \\sim Ueq, Uanis(C00M) \\sim Ueq, Uanis(C00N) \\sim Ueq,
Uanis(C00O) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C00Q) \\sim Ueq, Uanis(C00R)
\\sim Ueq, Uanis(C00S) \\sim Ueq, Uanis(C00T) \\sim Ueq, Uanis(C00U) \\sim Ueq,
Uanis(C00V) \\sim Ueq, Uanis(C00W) \\sim Ueq, Uanis(C00X) \\sim Ueq,
Uanis(C00Y) \\sim Ueq, Uanis(C00Z) \\sim Ueq, Uanis(C010) \\sim Ueq,
Uanis(C011) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C013) \\sim Ueq, Uanis(C014)
\\sim Ueq, Uanis(C015) \\sim Ueq, Uanis(C016) \\sim Ueq, Uanis(C017) \\sim Ueq,
Uanis(C018) \\sim Ueq, Uanis(C019) \\sim Ueq, Uanis(C01A) \\sim Ueq,
Uanis(C01B) \\sim Ueq, Uanis(C01C) \\sim Ueq, Uanis(C01D) \\sim Ueq,
Uanis(C01E) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C01G) \\sim Ueq, Uanis(C01H)
\\sim Ueq, Uanis(C01I) \\sim Ueq, Uanis(C01J) \\sim Ueq, Uanis(C01K) \\sim Ueq,
Uanis(C01L) \\sim Ueq, Uanis(C01M) \\sim Ueq, Uanis(C01N) \\sim Ueq,
Uanis(C01O) \\sim Ueq, Uanis(C01P) \\sim Ueq, Uanis(C01Q) \\sim Ueq,
Uanis(C01R) \\sim Ueq, Uanis(C01S) \\sim Ueq, Uanis(C01T) \\sim Ueq,
Uanis(C01U) \\sim Ueq, Uanis(C01V) \\sim Ueq, Uanis(C01W) \\sim Ueq,
Uanis(C01X) \\sim Ueq, Uanis(C01Y) \\sim Ueq, Uanis(C01Z) \\sim Ueq,
Uanis(C020) \\sim Ueq, Uanis(C021) \\sim Ueq, Uanis(C022) \\sim Ueq,
Uanis(C023) \\sim Ueq, Uanis(C024) \\sim Ueq, Uanis(C025) \\sim Ueq,
Uanis(C026) \\sim Ueq, Uanis(C027) \\sim Ueq, Uanis(C028) \\sim Ueq,
Uanis(C029) \\sim Ueq, Uanis(C02A) \\sim Ueq, Uanis(C02B) \\sim Ueq,
Uanis(C02C) \\sim Ueq, Uanis(C02D) \\sim Ueq, Uanis(C02E) \\sim Ueq,
Uanis(C02F) \\sim Ueq, Uanis(C02G) \\sim Ueq, Uanis(C02H) \\sim Ueq,
Uanis(C02I) \\sim Ueq, Uanis(C02J) \\sim Ueq, Uanis(C02K) \\sim Ueq,
Uanis(C02L) \\sim Ueq, Uanis(C02M) \\sim Ueq, Uanis(C02N) \\sim Ueq,
Uanis(C02O) \\sim Ueq, Uanis(C02P) \\sim Ueq, Uanis(C02Q) \\sim Ueq,
Uanis(C02R) \\sim Ueq, Uanis(C02S) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
3.a Ternary CH refined with riding coordinates:
 N1(H1), N3(H3), N2(H2), N4(H4)
3.b Secondary CH2 refined with riding coordinates:
 C00O(H00A,H00B), C00U(H00E,H00F), C00V(H00G,H00H), C00Y(H00C,H00D), C00Z(H00I,
 H00J), C016(H01A,H01B), C01Q(H01T,H01V), C01V(H01E,H01F)
3.c Aromatic/amide H refined with riding coordinates:
 C00X(H00X), C011(H011), C013(H013), C014(H014), C015(H015), C017(H017),
 C01A(H01G), C01B(H01H), C01C(H01C), C01D(H01D), C01E(H01I), C01G(H01K),
 C01H(H01M), C01I(H01O), C01J(H01J), C01K(H01Q), C01L(H01L), C01N(H01N),
 C01O(H01S), C01P(H01P), C01R(H01R), C01T(H01W), C01U(H01U), C01W(H01X),
 C01X(H01Y), C01Y(H01Z), C01Z(H01), C020(H020), C021(H021), C022(H022),
 C023(H023), C024(H024), C025(H025), C026(H026), C027(H027), C028(H028),
 C029(H029), C02A(H02A), C02B(H02B), C02C(H02C), C02D(H02D), C02E(H02E),
 C02F(H02F), C02G(H02G), C02H(H02H), C02I(H02I), C02J(H02J), C02K(H02K),
 C02L(H02L), C02M(H02M), C02N(H02N), C02O(H02O), C02P(H02P), C02Q(H02Q),
 C02R(H02R), C02S(H02S)
;
_shelx_res_checksum              45270
_shelx_hkl_checksum              75254
_olex2_submission_special_instructions 'No special instructions were received'