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_7701195
_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 H57 Mn N2 O3 P, C F3 O3 S'
_chemical_formula_sum            'C40 H57 F3 Mn N2 O6 P S'
_chemical_formula_weight         836.84
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-09-15
_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                85.551(5)
_cell_angle_beta                 89.809(4)
_cell_angle_gamma                76.872(4)
_cell_formula_units_Z            4
_cell_length_a                   10.7958(5)
_cell_length_b                   19.6144(10)
_cell_length_c                   20.0400(11)
_cell_measurement_reflns_used    7413
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      25.7290
_cell_measurement_theta_min      3.2700
_cell_volume                     4119.7(4)
_computing_cell_refinement
'CrysAlisPro, Agilent Technologies, Version 1.171.37.34k (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,16:31:05)'
_computing_data_collection
'CrysAlisPro, Agilent Technologies, Version 1.171.37.34k (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,16:31:05)'
_computing_data_reduction
'CrysAlisPro, Agilent Technologies, Version 1.171.37.34k (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,16:31:05)'
_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      120.00(10)
_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 0.993
_diffrn_measurement_details
;
  1 omega  -20.00   33.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       -7.3914  -99.0000 -120.0000 53

  2 omega  -20.00   33.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       -7.3914  -99.0000  -60.0000 53

  3 omega  -69.00   13.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       -7.3914  -57.0000 -120.0000 82

  4 omega  -85.00   22.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       -7.3914  -19.0000  120.0000 107

  5 omega  -11.00   16.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       -7.3914  -99.0000  120.0000 27

  6 omega  -30.00   65.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       -7.3914   38.0000   90.0000 95

  7 omega  -13.00   14.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       -7.3914  -38.0000 -180.0000 27

  8 omega   -5.00   29.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       -7.3914  -99.0000  -90.0000 34

  9 omega   27.00   54.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -        8.4852   38.0000 -120.0000 27

 10 omega  -21.00    4.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -        8.4852  -77.0000  120.0000 25

 11 omega   32.00   59.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -        8.4852   77.0000   90.0000 27

 12 omega  -20.00    7.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -        8.4852   77.0000   90.0000 27
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0630841000
_diffrn_orient_matrix_UB_12      -0.0206284000
_diffrn_orient_matrix_UB_13      0.0034455000
_diffrn_orient_matrix_UB_21      0.0217310000
_diffrn_orient_matrix_UB_22      0.0300831000
_diffrn_orient_matrix_UB_23      0.0075544000
_diffrn_orient_matrix_UB_31      -0.0100306000
_diffrn_orient_matrix_UB_32      -0.0075461000
_diffrn_orient_matrix_UB_33      0.0345205000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1038
_diffrn_reflns_av_unetI/netI     0.1049
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -3
_diffrn_reflns_number            15033
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.394
_diffrn_reflns_theta_min         2.792
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.471
_exptl_absorpt_correction_T_max  0.937
_exptl_absorpt_correction_T_min  0.702
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
'CrysAlisPro, Agilent Technologies, Version 1.171.37.34k (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,16:31:05) 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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.349
_exptl_crystal_description       block
_exptl_crystal_F_000             1768
_exptl_crystal_recrystallization_method
'The material was recrystallised from a mixture of pentane and acetone by vapour diffusion'
_exptl_crystal_size_max          0.3664
_exptl_crystal_size_mid          0.1225
_exptl_crystal_size_min          0.0688
_refine_diff_density_max         2.083
_refine_diff_density_min         -0.823
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1105
_refine_ls_number_reflns         15033
_refine_ls_number_restraints     195
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.1283
_refine_ls_R_factor_gt           0.0920
_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^)+(0.0556P)^2^+17.6221P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1981
_refine_ls_wR_factor_ref         0.2169
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10823
_reflns_number_total             15033
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03100f2.cif
_cod_data_source_block           ex4010
_cod_depositor_comments
'Adding full bibliography for 7701195--7701196.cif.'
_cod_database_code               7701195
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'C40 H57 F3 Mn N2 O6 P S'
_chemical_oxdiff_usercomment     '@ 120 K sample 4'
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_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. Shared sites
{O55, O56'}
3. Restrained distances
 P51-C78 \\sim P51-C84
 with sigma of 0.02
 P51-C78' \\sim P51-C84
 with sigma of 0.02
 C83-C78 \\sim C89-C84
 with sigma of 0.02
 C83-C82' \\sim C89-C88
 with sigma of 0.02
 C82'-C81' \\sim C88-C87
 with sigma of 0.02
 C81'-C80' \\sim C87-C86
 with sigma of 0.02
 C80'-C79' \\sim C86-C85
 with sigma of 0.02
 C79'-C78 \\sim C85-C84
 with sigma of 0.02
 C83'-C78' \\sim C89-C84
 with sigma of 0.02
 C83'-C82 \\sim C89-C88
 with sigma of 0.02
 C82-C81 \\sim C88-C87
 with sigma of 0.02
 C81-C80 \\sim C87-C86
 with sigma of 0.02
 C80-C79 \\sim C86-C85
 with sigma of 0.02
 C79-C78' \\sim C85-C84
 with sigma of 0.02
 C82-C80 \\sim C88-C86
 with sigma of 0.02
4. Rigid bond restraints
 O5, S1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
O5 \\sim S1: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(O55) = Uanis(O56')
6. Rigid body (RIGU) restrains
 C78, C78', C79, C79', C80, C80', C81, C81', C82, C82', C83, C83'
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S51', O54', O55', O56', F51', F52', F53', C91'
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O5, S1, O4, O6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Same fragment restrains
{S51, F51, F52, F53, O54, O55, O56, C91}
as
{S51', F51', F52', F53', O54', O55', O56', C91'}
8. Others
 Sof(C78')=Sof(H78')=Sof(C79)=Sof(H79A)=Sof(H79B)=Sof(C80)=Sof(H80A)=Sof(H80B)=
 Sof(C81)=Sof(H81A)=Sof(H81B)=Sof(C82)=Sof(H82A)=Sof(H82B)=Sof(C83')=Sof(H83C)=
 Sof(H83D)=1-FVAR(1)
 Sof(C78)=Sof(H78)=Sof(C79')=Sof(H79C)=Sof(H79D)=Sof(C80')=Sof(H80C)=Sof(H80D)=
 Sof(C81')=Sof(H81C)=Sof(H81D)=Sof(C82')=Sof(H82C)=Sof(H82D)=Sof(C83)=Sof(H83A)=
 Sof(H83B)=FVAR(1)
 Sof(S51')=Sof(F51')=Sof(F52')=Sof(F53')=Sof(O54')=Sof(O55')=Sof(O56')=
 Sof(C91')=1-FVAR(2)
 Sof(S51)=Sof(F51)=Sof(F52)=Sof(F53)=Sof(O54)=Sof(O55)=Sof(O56)=Sof(C91)=FVAR(2)
9.a Ternary CH refined with riding coordinates:
 C72(H72), C78(H78), C78'(H78'), C84(H84), C22(H22), C28(H28), C34(H34)
9.b Secondary CH2 refined with riding coordinates:
 C73(H73A,H73B), C74(H74A,H74B), C75(H75A,H75B), C76(H76A,H76B), C77(H77A,
 H77B), C79(H79A,H79B), C79'(H79C,H79D), C80(H80A,H80B), C80'(H80C,H80D),
 C81(H81A,H81B), C81'(H81C,H81D), C82(H82A,H82B), C82'(H82C,H82D), C83(H83A,
 H83B), C83'(H83C,H83D), C85(H85A,H85B), C86(H86A,H86B), C87(H87A,H87B),
 C88(H88A,H88B), C89(H89A,H89B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B),
  C26(H26A,H26B), C27(H27A,H27B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,
 H31B), C32(H32A,H32B), C33(H33A,H33B), C35(H35A,H35B), C36(H36A,H36B),
 C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B)
9.c Aromatic/amide H refined with riding coordinates:
 C51(H51), C52(H52), C54(H54), C57(H57), C59(H59), C60(H60), C1(H1), C2(H2),
 C4(H4), C7(H7), C9(H9), C10(H10)
9.d Idealised Me refined as rotating group:
 C62(H62A,H62B,H62C), C63(H63A,H63B,H63C), C64(H64A,H64B,H64C), C66(H66A,H66B,
 H66C), C67(H67A,H67B,H67C), C68(H68A,H68B,H68C), C12(H12A,H12B,H12C), C13(H13A,
 H13B,H13C), C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C),
 C18(H18A,H18B,H18C)
;
_shelx_res_checksum              16979
_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 4'
_olex2_submission_special_instructions 'No special instructions were received'