Inter-ligand intramolecular through-space anisotropic shielding in a series of manganese carbonyl phosphorous compounds.
Kurtz, Daniel A.; Dhakal, Badrinath; McDonald, Lauren T.; Nichol, Gary S.; Felton, Greg A. N.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 14926–14935; doi:10.1039/c9dt03100f

data_7701196
_publ_section_title
;
 Inter-ligand intramolecular through-space anisotropic shielding in a
 series of manganese carbonyl phosphorous compounds.
;
_journal_issue                   39
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14926
_journal_page_last               14935
_journal_paper_doi               10.1039/c9dt03100f
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C39 H39 Mn N2 O3 P, C F3 O3 S'
_chemical_formula_sum            'C40 H39 F3 Mn N2 O6 P S'
_chemical_formula_weight         818.70
_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     direct
_audit_creation_date             2014-09-17
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2014.08.28 svn.r2986 for OlexSys, GUI svn.r4874)
;
_audit_update_record
;
2019-06-03 deposited with the CCDC.    2019-09-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.524(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   37.1455(10)
_cell_length_b                   10.5546(3)
_cell_length_c                   20.3195(5)
_cell_measurement_reflns_used    15745
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      30.0310
_cell_measurement_theta_min      3.3700
_cell_volume                     7856.6(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1574
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -20.00   27.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.2412  -99.0000 -180.0000 47

  2 omega  -92.00   24.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.2412  -19.0000  -30.0000 116

  3 omega  -86.00    9.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.2412  -38.0000  -90.0000 95

  4 omega  -45.00   61.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.2412   77.0000 -120.0000 106

  5 omega  -20.00   54.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       14.3350  -99.0000 -150.0000 74

  6 omega   35.00  101.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       14.3350  178.0000 -150.0000 66

  7 omega  -86.00    9.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.2412  -38.0000   90.0000 95

  8 omega  -36.00   59.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.2412   38.0000   30.0000 95

  9 omega  -56.00  -11.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       14.3350  -57.0000   60.0000 45
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Agilent Technologies SuperNova'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0074404000
_diffrn_orient_matrix_UB_12      -0.0210079000
_diffrn_orient_matrix_UB_13      -0.0325675000
_diffrn_orient_matrix_UB_21      0.0170548000
_diffrn_orient_matrix_UB_22      0.0105682000
_diffrn_orient_matrix_UB_23      -0.0104268000
_diffrn_orient_matrix_UB_31      0.0053466000
_diffrn_orient_matrix_UB_32      -0.0629590000
_diffrn_orient_matrix_UB_33      0.0091374000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0666
_diffrn_reflns_av_unetI/netI     0.0354
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            69991
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         2.846
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.492
_exptl_absorpt_correction_T_max  0.829
_exptl_absorpt_correction_T_min  0.589
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
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            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.384
_exptl_crystal_description       block
_exptl_crystal_F_000             3392
_exptl_crystal_recrystallization_method
'The material was recrystallised from a mixture of pentane and acetone by vapour diffusion'
_exptl_crystal_size_max          0.256
_exptl_crystal_size_mid          0.125
_exptl_crystal_size_min          0.0809
_refine_diff_density_max         0.426
_refine_diff_density_min         -0.348
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     597
_refine_ls_number_reflns         8027
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0566
_refine_ls_R_factor_gt           0.0437
_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^)+(0.0387P)^2^+16.4268P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1004
_refine_ls_wR_factor_ref         0.1069
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6611
_reflns_number_total             8027
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03100f2.cif
_cod_data_source_block           ex4012
_cod_depositor_comments
'Adding full bibliography for 7701195--7701196.cif.'
_cod_database_code               7701196
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'C40 H39 F3 Mn N2 O6 P S'
_chemical_oxdiff_usercomment     '@ 120 K sample 5'
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 C11', C15', C14', C13', C3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Same fragment restrains
{C15, C16, C17, C18}
as
{C11, C12, C13, C14}
{C15, C16, C17, C18}
as
{C11', C13', C14', C15'}
4. Others
 Sof(S004)=Sof(F1')=Sof(F2')=Sof(F3')=Sof(O4')=Sof(O5')=Sof(O6')=1-FVAR(1)
 Sof(S1)=Sof(F1)=Sof(F2)=Sof(F3)=Sof(O4)=Sof(O5)=Sof(O6)=FVAR(1)
 Sof(C11')=Sof(C13')=Sof(H13D)=Sof(H13E)=Sof(H13F)=Sof(C14')=Sof(H14D)=
 Sof(H14E)=Sof(H14F)=Sof(C15')=Sof(H15A)=Sof(H15B)=Sof(H15C)=1-FVAR(2)
 Sof(C11)=Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(H12C)=Sof(C13)=Sof(H13A)=Sof(H13B)=
 Sof(H13C)=Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=FVAR(2)
5.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C7(H7), C9(H9), C10(H10), C23(H23), C24(H24),
 C25(H25), C26(H26), C27(H27), C29(H29), C30(H30), C31(H31), C32(H32), C33(H33),
  C35(H35), C36(H36), C37(H37), C38(H38), C39(H39)
5.b Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C13'(H13D,H13E,
 H13F), C14'(H14D,H14E,H14F), C15'(H15A,H15B,H15C), C16(H16A,H16B,H16C),
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C)
;
_shelx_res_checksum              7099
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems Cryostream 700+'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in Paratone oil'
_olex2_submission_original_sample_id 'sample 5'
_olex2_submission_special_instructions 'No special instructions were received'