Bisphosphine phenol and phenolate complexes of Mn(i): manganese(i) catalyzed Tishchenko reaction.
Kadassery, Karthika J.; MacMillan, Samantha N.; Lacy, David C.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 12652–12655; doi:10.1039/c8dt02933d

data_7047256
_publ_section_title
;
 Bisphosphine phenol and phenolate complexes of Mn(i): manganese(i)
 catalyzed Tishchenko reaction.
;
_journal_issue                   36
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12652
_journal_page_last               12655
_journal_paper_doi               10.1039/c8dt02933d
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C72 H58 Mn2 O8 P4, 6(C4 H8 O)'
_chemical_formula_sum            'C96 H106 Mn2 O14 P4'
_chemical_formula_weight         1717.56
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-08-03
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-08-07 deposited with the CCDC.
2018-08-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 114.095(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.0462(5)
_cell_length_b                   14.1147(2)
_cell_length_c                   25.4480(5)
_cell_measurement_reflns_used    27056
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      31.6590
_cell_measurement_theta_min      2.1390
_cell_volume                     8540.4(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_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_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     16.00  42.00   0.50   20.50    --    5.32  37.00  60.00   52
  2  \w      6.00  35.00   0.50   20.50    --    5.32-100.00  68.00   58
  3  \w    -24.00  25.00   0.50   20.50    --   -6.42-100.00  68.00   98
  4  \w    -26.00  37.00   0.50   20.50    --    5.32 -99.00  30.00  126
  5  \w    -23.00  23.00   0.50   20.50    --    5.32 -99.00 -90.00   92
  6  \w    -16.00  26.00   0.50   20.50    --   -6.42 -99.00-180.00   84
  7  \w    -26.00  26.00   0.50   20.50    --   -6.42 -99.00-120.00  104
  8  \w    -66.00   0.00   0.50   20.50    --    5.32 -37.00-150.00  132
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0257496000
_diffrn_orient_matrix_UB_12      0.0248940000
_diffrn_orient_matrix_UB_13      -0.0135611000
_diffrn_orient_matrix_UB_21      -0.0149436000
_diffrn_orient_matrix_UB_22      -0.0407853000
_diffrn_orient_matrix_UB_23      0.0020885000
_diffrn_orient_matrix_UB_31      0.0019797000
_diffrn_orient_matrix_UB_32      0.0154922000
_diffrn_orient_matrix_UB_33      0.0272840000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0251
_diffrn_reflns_av_unetI/netI     0.0173
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            51384
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.103
_diffrn_reflns_theta_min         1.886
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.436
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.409
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.29d (Rigaku Oxford Diffraction, 2017)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_density_diffrn    1.336
_exptl_crystal_description       block
_exptl_crystal_F_000             3616
_exptl_crystal_size_max          0.291
_exptl_crystal_size_mid          0.167
_exptl_crystal_size_min          0.164
_refine_diff_density_max         0.609
_refine_diff_density_min         -0.774
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     570
_refine_ls_number_reflns         9407
_refine_ls_number_restraints     236
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0465
_refine_ls_R_factor_gt           0.0409
_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^)+(0.0649P)^2^+16.4297P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1140
_refine_ls_wR_factor_ref         0.1186
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8320
_reflns_number_total             9407
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02933d2.cif
_cod_data_source_block           rlacy8_abs
_cod_depositor_comments
'Adding full bibliography for 7047253--7047256.cif.'
_cod_database_code               7047256
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         MnO7P2C48H53
_chemical_oxdiff_usercomment     'Crystallized from THF/hexanes.'
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.04
_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. Uiso/Uaniso restraints and constraints
O7 \\sim C45 \\sim C46 \\sim C47 \\sim C48 \\sim O7A \\sim C45A \\sim C46A
\\sim C47A \\sim C48A: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
3. Rigid body (RIGU) restrains
 O7, C45, C46, C47, C48, O7A, C45A, C46A, C47A, C48A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Same fragment restrains
{O7, C45, C46, C47, C48} sigma for 1-2: 0.02, 1-3: 0.04
{O7A, C48A, C47A, C46A, C45A} sigma for 1-2: 0.02, 1-3: 0.04
as
{O7A, C45A, C46A, C47A, C48A}
5. Others
 Sof(O7A)=Sof(C45A)=Sof(H45C)=Sof(H45D)=Sof(C46A)=Sof(H46C)=Sof(H46D)=
 Sof(C47A)=Sof(H47C)=Sof(H47D)=Sof(C48A)=Sof(H48C)=Sof(H48D)=1-FVAR(1)
 Sof(O7)=Sof(C45)=Sof(H45A)=Sof(H45B)=Sof(C46)=Sof(H46A)=Sof(H46B)=Sof(C47)=
 Sof(H47A)=Sof(H47B)=Sof(C48)=Sof(H48A)=Sof(H48B)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C23(H23A,H23B), C45(H45A,H45B), C46(H46A,H46B), C47(H47A,
 H47B), C48(H48A,H48B), C45A(H45C,H45D), C46A(H46C,H46D), C47A(H47C,H47D),
 C48A(H48C,H48D), C41(H41A,H41B), C42(H42A,H42B), C43(H43A,H43B), C44(H44A,
 H44B), C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B)
6.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C11(H11), C12(H12), C13(H13),
 C14(H14), C15(H15), C18(H18), C20(H20), C25(H25), C26(H26), C27(H27), C28(H28),
  C29(H29), C31(H31), C32(H32), C33(H33), C34(H34), C35(H35)
6.c Idealised Me refined as rotating group:
 C36(H36A,H36B,H36C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.224
_oxdiff_exptl_absorpt_empirical_full_min 0.891