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_7047253
_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         'C36 H29 Mn O4 P2, 2(C H2 Cl2)'
_chemical_formula_sum            'C38 H33 Cl4 Mn O4 P2'
_chemical_formula_weight         812.32
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 101.206(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.5689(3)
_cell_length_b                   12.6052(2)
_cell_length_c                   18.8201(3)
_cell_measurement_reflns_used    23320
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      31.4260
_cell_measurement_theta_min      1.8730
_cell_volume                     3623.01(11)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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     -8.00  69.00   0.50    3.00    --    5.32  57.00   0.00  154
  2  \w    -67.00  64.00   0.50    3.00    --    5.32   0.00   0.00  262
  3  \w    -67.00  16.00   0.50    3.00    --    5.32 -37.00 150.00  166
  4  \w      4.00  36.00   0.50    3.00    --    5.32 -99.00 150.00   64
  5  \w    -21.00   4.00   0.50    3.00    --   -6.42 -99.00 -90.00   50
;
_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      -0.0051842000
_diffrn_orient_matrix_UB_12      -0.0074983000
_diffrn_orient_matrix_UB_13      -0.0379450000
_diffrn_orient_matrix_UB_21      -0.0015573000
_diffrn_orient_matrix_UB_22      -0.0557136000
_diffrn_orient_matrix_UB_23      0.0049328000
_diffrn_orient_matrix_UB_31      -0.0461212000
_diffrn_orient_matrix_UB_32      0.0027492000
_diffrn_orient_matrix_UB_33      -0.0034113000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0294
_diffrn_reflns_av_unetI/netI     0.0211
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            41198
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.103
_diffrn_reflns_theta_min         1.889
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.788
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.346
_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    1.489
_exptl_crystal_description       block
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.318
_exptl_crystal_size_mid          0.218
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.523
_refine_diff_density_min         -1.080
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     443
_refine_ls_number_reflns         7972
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0448
_refine_ls_R_factor_gt           0.0402
_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^)+(0.0486P)^2^+5.8279P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1040
_refine_ls_wR_factor_ref         0.1066
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7147
_reflns_number_total             7972
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02933d2.cif
_cod_data_source_block           rlacy7_abs
_cod_depositor_comments
'Adding full bibliography for 7047253--7047256.cif.'
_cod_database_code               7047253
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C38H36Cl4MnO4P2
_chemical_oxdiff_usercomment     'Crystallized from DCM/ether.'
_reflns_odcompleteness_completeness 99.93
_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.a Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C23(H23A,H23B), C37(H37A,H37B), C38(H38A,H38B)
2.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)
2.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 1.236
_oxdiff_exptl_absorpt_empirical_full_min 0.923