A hemilabile manganese(I)-phenol complex and its coordination induced O-H bond weakening.
Kadassery, Karthika J.; Crawley, Matthew R.; MacMillan, Samantha N.; Lacy, David C.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 16217–16225; doi:10.1039/d0dt00973c

data_7704185
_publ_section_title
;
 A hemilabile manganese(I)-phenol complex and its coordination induced O-H
 bond weakening.
;
_journal_issue                   45
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16217
_journal_page_last               16225
_journal_paper_doi               10.1039/d0dt00973c
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C44 H41 Mn O4 P2'
_chemical_formula_sum            'C44 H41 Mn O4 P2'
_chemical_formula_weight         750.65
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-07-29
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2020-03-02 deposited with the CCDC.	2020-04-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.1990(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.27050(10)
_cell_length_b                   38.3219(3)
_cell_length_c                   9.61390(10)
_cell_measurement_reflns_used    30155
_cell_measurement_temperature    253.00(10)
_cell_measurement_theta_max      76.9670
_cell_measurement_theta_min      2.2980
_cell_volume                     3735.22(6)
_computing_cell_refinement       'CrysAlisPro 1.171.40.58a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.58a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.58a (Rigaku OD, 2019)'
_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      253.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.991
_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    -14.00  18.00   0.50    1.34    --  -50.06  95.00-113.00   64
  2  \w    -74.00 -17.00   0.50    1.34    --  -50.06  95.00-113.00  114
  3  \w    -69.00 -44.00   0.50    5.35    --  -82.50  95.00-113.00   50
  4  \w    -97.00 -46.00   0.50    1.34    --  -50.06   0.00  60.00  102
  5  \w    -51.00 -13.00   0.50    5.35    --  -82.50  45.00  90.00   76
  6  \w     -6.00  43.00   0.50    1.34    --   50.06 -95.00 136.00   98
  7  \w     33.00 100.00   0.50    5.35    --  104.00 -95.00 136.00  134
  8  \w     75.00 101.00   0.50    5.35    --  104.00-125.00  90.00   52
  9  \w     73.00  99.00   0.50    5.35    --  104.00 -94.00  90.00   52
 10  \w     71.00  97.00   0.50    5.35    --  104.00 -77.00  60.00   52
 11  \w     78.00 107.00   0.50    5.35    --  104.00-105.00  22.78   58
 12  \w     64.00  91.00   0.50    5.35    --  104.00 -77.00 -30.00   54
 13  \w     81.00 106.00   0.50    5.35    --  104.00 -94.00 -90.00   50
 14  \w     50.00  91.00   0.50    5.35    --  104.00 -77.00   0.00   82
 15  \w     48.00  73.00   0.50    5.35    --  104.00-105.00  22.78   50
 16  \w     44.00  71.00   0.50    5.35    --  104.00 -61.00   0.00   54
 17  \w     33.00  62.00   0.50    5.35    --  104.00 -59.00  29.05   58
 18  \w     33.00  58.00   0.50    5.35    --  104.00 -94.00  90.00   50
 19  \w     59.00  85.00   0.50    5.35    --  104.00 -77.00  90.00   52
 20  \w     71.00 105.00   0.50    5.35    --  104.00 -94.00 150.00   68
 21  \w     59.00 121.00   0.50    5.35    --  104.00 -81.00 171.57  124
 22  \w    111.00 138.00   0.50    5.35    --  104.00  15.00  60.00   54
 23  \w    137.00 175.00   0.50    5.35    --  104.00  30.00  30.00   76
 24  \w    149.00 174.00   0.50    5.35    --  104.00  61.00 120.00   50
 25  \w    117.00 142.00   0.50    5.35    --  104.00  61.00 120.00   50
 26  \w    101.00 131.00   0.50    5.35    --  104.00  30.00  30.00   60
 27  \w    108.00 136.00   0.50    5.35    --  104.00  61.00 -60.00   56
 28  \w    141.00 166.00   0.50    5.35    --  104.00  61.00 -60.00   50
 29  \w    136.00 165.00   0.50    5.35    --  104.00  45.00 -90.00   58
 30  \w    128.00 154.00   0.50    5.35    --  104.00  93.00 -97.15   52
 31  \w    149.00 176.00   0.50    5.35    --  104.00  96.00 -43.90   54
 32  \w    134.00 176.00   0.50    5.35    --  104.00 125.00 -30.00   84
 33  \w    118.00 146.00   0.50    5.35    --  104.00  95.00-113.00   56
 34  \w    120.00 146.00   0.50    5.35    --  104.00  61.00-180.00   52
 35  \w    149.00 175.00   0.50    5.35    --  104.00  61.00-180.00   52
 36  \w    111.00 137.00   0.50    5.35    --  104.00  30.00-180.00   52
 37  \w     96.00 126.00   0.50    5.35    --  104.00  45.00 -90.00   60
 38  \w    100.00 133.00   0.50    5.35    --  104.00  15.00 -60.00   66
 39  \w     96.00 126.00   0.50    5.35    --  104.00 125.00 -30.00   60
 40  \w     56.00 110.00   0.50    5.35    --  104.00   0.00 -90.00  108
 41  \w     32.00  57.00   0.50    5.35    --  104.00 -61.00-150.00   50
 42  \w     38.00  64.00   0.50    5.35    --  104.00 -61.00-120.00   52
 43  \w     38.00  64.00   0.50    5.35    --  104.00 -63.00-102.22   52
 44  \w     33.00  59.00   0.50    5.35    --  104.00 -77.00-120.00   52
 45  \w     39.00 104.00   0.50    5.35    --  104.00-116.00-159.34  130
 46  \w     35.00  91.00   0.50    5.35    --  104.00-125.00 -90.00  112
 47  \w     35.00  61.00   0.50    5.35    --  104.00 -77.00 -30.00   52
 48  \w     34.00  61.00   0.50    5.35    --  104.00 -94.00 -90.00   54
 49  \w     35.00  70.00   0.50    5.35    --  104.00 -61.00 -60.00   70
 50  \w     34.00  66.00   0.50    5.35    --  104.00 -77.00  60.00   64
 51  \w     32.00  90.00   0.50    5.35    --  104.00-120.00 124.06  116
 52  \w    -19.00  27.00   0.50    1.34    --   50.06 -19.00-120.00   92
 53  \w   -120.00 -74.00   0.50    1.34    --  -50.06-125.00-150.00   92
 54  \w   -118.00 -74.00   0.50    1.34    --  -50.06-125.00 -60.00   88
 55  \w   -143.00-118.00   0.50    5.35    --  -82.50 -95.00 136.00   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      0.0574330000
_diffrn_orient_matrix_UB_12      -0.0368375000
_diffrn_orient_matrix_UB_13      -0.0112202000
_diffrn_orient_matrix_UB_21      -0.0179526000
_diffrn_orient_matrix_UB_22      -0.0075826000
_diffrn_orient_matrix_UB_23      0.1531715000
_diffrn_orient_matrix_UB_31      -0.1395092000
_diffrn_orient_matrix_UB_32      -0.0142088000
_diffrn_orient_matrix_UB_33      -0.0525896000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0322
_diffrn_reflns_av_unetI/netI     0.0211
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       48
_diffrn_reflns_limit_k_min       -48
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            55421
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.104
_diffrn_reflns_theta_min         2.306
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.022
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.449
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.58a (Rigaku Oxford Diffraction, 2019)
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 orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.335
_exptl_crystal_description       plate
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.204
_exptl_crystal_size_mid          0.084
_exptl_crystal_size_min          0.038
_refine_diff_density_max         0.252
_refine_diff_density_min         -0.265
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     467
_refine_ls_number_reflns         7822
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_gt           0.0336
_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^)+(0.0359P)^2^+1.8181P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0809
_refine_ls_wR_factor_ref         0.0846
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7312
_reflns_number_total             7822
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00973c3.cif
_cod_data_source_block           rlacy36_abs
_cod_depositor_comments
'Adding full bibliography for 7704185--7704186.cif.'
_cod_database_code               7704185
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C44H41MnO4P2
_chemical_oxdiff_usercomment     'Crystallized from CH2Cl2/pentanes.'
_reflns_odcompleteness_completeness 97.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     77.83
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O3-H3
 0.82 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C36(H36A,H36B)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3A), C4(H4), C5(H5), C6(H6), C7(H7), C10(H10), C11(H11), C12(H12),
 C13(H13), C14(H14), C17(H17), C19(H19), C24(H24), C25(H25), C26(H26), C27(H27),
  C28(H28), C31(H31), C32(H32), C33(H33), C34(H34), C35(H35), C38(H38), C40(H40)
3.c Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C43(H43A,H43B,H43C), C44(H44A,H44B,
 H44C)
;
_shelx_res_checksum              76106
_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 1.203
_oxdiff_exptl_absorpt_empirical_full_min 0.847