Reactions of [(dmpe)<sub>2</sub>MnH(C<sub>2</sub>H<sub>4</sub>)]: synthesis and characterization of manganese(i) borohydride and hydride complexes.
Price, Jeffrey S.; DeJordy, Declan M.; Emslie, David J. H.; Britten, James F.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 9983–9994; doi:10.1039/d0dt01726d

data_7704765
_publ_section_title
;
 Reactions of [(dmpe)<sub>2</sub>MnH(C<sub>2</sub>H<sub>4</sub>)]:
 synthesis and characterization of manganese(i) borohydride and hydride
 complexes.
;
_journal_issue                   29
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9983
_journal_page_last               9994
_journal_paper_doi               10.1039/d0dt01726d
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C30 H80.84 Mn2 P10'
_chemical_formula_sum            'C30 H82 Mn2 P10'
_chemical_formula_weight         862.53
_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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2019-04-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-05-08 deposited with the CCDC.	2020-06-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.652(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.392(2)
_cell_length_b                   10.4309(14)
_cell_length_c                   28.529(4)
_cell_measurement_reflns_used    5034
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.584
_cell_measurement_theta_min      2.416
_cell_volume                     4528.3(11)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0898
_diffrn_reflns_av_unetI/netI     0.0918
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            56722
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.200
_diffrn_reflns_theta_min         1.338
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.931
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6658
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 'SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.0645 before and 0.0542 after correction.
The Ratio of minimum to maximum transmission is 0.8927.
The \l/2 correction factor is 0.00150.'
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.265
_exptl_crystal_description       block
_exptl_crystal_F_000             1848
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.143
_exptl_crystal_size_min          0.125
_refine_diff_density_max         2.297
_refine_diff_density_min         -1.355
_refine_diff_density_rms         0.241
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     486
_refine_ls_number_reflns         12351
_refine_ls_number_restraints     870
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.1648
_refine_ls_R_factor_gt           0.1092
_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^)+(0.1569P)^2^+41.3264P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2817
_refine_ls_wR_factor_ref         0.3234
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7949
_reflns_number_total             12351
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01726d3.cif
_cod_data_source_block           MnHdmpe_bridging_cis
_cod_depositor_comments
'Adding full bibliography for 7704762--7704768.cif.'
_cod_original_cell_volume        4528.2(10)
_cod_database_code               7704765
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.893
_shelx_estimated_absorpt_t_min   0.787
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.9415(11)
 0.0585(11)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C30A-P10A
 1.85 with sigma of 0.02
 C29A-P10A
 1.85 with sigma of 0.02
 C24A-P8A
 1.85 with sigma of 0.02
 P5A-C14A
 1.85 with sigma of 0.02
 C13A-P5A
 1.85 with sigma of 0.02
 C15A-P5A
 1.85 with sigma of 0.02
 C15A-C16A
 1.55 with sigma of 0.02
 C5A-P2A
 1.85 with sigma of 0.02
 P3A-C8A
 1.85 with sigma of 0.02
 C7A-C8A
 2.8 with sigma of 0.02
 C5A-C6A
 2.8 with sigma of 0.02
 C4A-C5A
 2.81 with sigma of 0.02
 C4A-C6A
 2.81 with sigma of 0.02
 C9A-C7A
 2.81 with sigma of 0.02
 C9A-C8A
 2.81 with sigma of 0.02
 C1A-C3A
 2.81 with sigma of 0.02
 C3A-C2A
 2.81 with sigma of 0.02
 C1A-C2A
 2.8 with sigma of 0.02
 C24A-C22A \\sim C22A-C23A \\sim C23A-C24A
 with sigma of 0.002
 C21A-C20A \\sim C20A-C19A \\sim C19A-C21A
 with sigma of 0.002
 C29A-C28A \\sim C28A-C30A \\sim C30A-C29A
 with sigma of 0.002
 C25A-C27A \\sim C27A-C26A \\sim C26A-C25A
 with sigma of 0.002
 C22A-C21A \\sim C27A-C28A \\sim C10A-C9A \\sim C15A-C16A
 with sigma of 0.002
 P10A-C28A \\sim P9A-C27A \\sim P8A-C22A \\sim P7A-C21A \\sim P3A-C9A
 with sigma of 0.002
 C30A-P10A \\sim C29A-P10A
 with sigma of 0.002
 C14A-C15A \\sim C15A-C13A \\sim C13A-C14A
 with sigma of 0.002
 C16A-C17A \\sim C17A-C18A \\sim C18A-C16A
 with sigma of 0.002
 C10A-C12A \\sim C12A-C11A \\sim C11A-C10A
 with sigma of 0.002
 C9A-C7A \\sim C7A-C8A \\sim C8A-C9A
 with sigma of 0.002
 C28A-C30A \\sim C30A-C29A \\sim C29A-C28A
 with sigma of 0.002
 C27A-C26A \\sim C26A-C25A \\sim C25A-C27A
 with sigma of 0.002
 C23A-C24A \\sim C24A-C22A \\sim C22A-C23A
 with sigma of 0.002
 C20A-C21A \\sim C21A-C19A \\sim C19A-C20A
 with sigma of 0.002
 C20A-P7A \\sim P7A-C19A
 with sigma of 0.002
4. Uiso/Uaniso restraints and constraints
Uanis(C10A) = Uanis(C9A)
Uanis(C28A) = Uanis(C27A)
Uanis(C3) = Uanis(C3A) = Uanis(C4A) = Uanis(C4)
Uanis(P7) = Uanis(P2A)
Uanis(P9A) = Uanis(P2)
Uanis(P10A) = Uanis(P9)
Uanis(P8) = Uanis(P7A)
Uanis(P8A) = Uanis(P10)
Uanis(P1) = Uanis(P3A)
Uanis(P4) = Uanis(P5A)
Uanis(P3) = Uanis(P4A)
Uanis(P6A) = Uanis(P5)
Uanis(P1A) = Uanis(P6)
Uanis(C21) = Uanis(C5A)
Uanis(C20) = Uanis(C4A)
Uanis(C6A) = Uanis(C19)
Uanis(C27A) = Uanis(C6)
Uanis(C21A) = Uanis(C23)
Uanis(C22A) = Uanis(C30)
Uanis(C5) = Uanis(C23A)
Uanis(C26A) = Uanis(C5)
Uanis(C27) = Uanis(C29A)
Uanis(C25) = Uanis(C30A) = Uanis(C26) = Uanis(C20A)
Uanis(C25A) = Uanis(C29)
Uanis(C24) = Uanis(C19A)
Uanis(C29) = Uanis(C24A)
Uanis(C1A) = Uanis(C17)
Uanis(C17) = Uanis(C1A)
Uanis(C2) = Uanis(C7A)
Uanis(C9A) = Uanis(C1)
Uanis(C12A) = Uanis(C7)
Uanis(C9) = Uanis(C11A)
Uanis(C16A) = Uanis(C14)
Uanis(C18A) = Uanis(C13)
Uanis(C17A) = Uanis(C8)
Uanis(C14A) = Uanis(C18)
Uanis(C13A) = Uanis(C11)
Uanis(C15A) = Uanis(C12)
Uanis(C2A) = Uanis(C16)
Uanis(C8A) = Uanis(C2)
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(P1A)=Sof(P2A)=Sof(P3A)=Sof(P4A)=Sof(P5A)=Sof(P6A)=Sof(P7A)=Sof(P8A)=
 Sof(P9A)=Sof(P10A)=Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(C2A)=Sof(H2AA)=
 Sof(H2AB)=Sof(H2AC)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(C4A)=Sof(H4AA)=Sof(H4AB)=
 Sof(C5A)=Sof(H5AA)=Sof(H5AB)=Sof(H5AC)=Sof(C6A)=Sof(H6AA)=Sof(H6AB)=Sof(H6AC)=
 Sof(C7A)=Sof(H7AA)=Sof(H7AB)=Sof(H7AC)=Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(H8AC)=
 Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(C10A)=Sof(H10C)=Sof(H10D)=Sof(C11A)=Sof(H11D)=
 Sof(H11E)=Sof(H11F)=Sof(C12A)=Sof(H12D)=Sof(H12E)=Sof(H12F)=Sof(C13A)=
 Sof(H13D)=Sof(H13E)=Sof(H13F)=Sof(C14A)=Sof(H14D)=Sof(H14E)=Sof(H14F)=
 Sof(C15A)=Sof(H15C)=Sof(H15D)=Sof(C16A)=Sof(H16C)=Sof(H16D)=Sof(C17A)=
 Sof(H17D)=Sof(H17E)=Sof(H17F)=Sof(C18A)=Sof(H18D)=Sof(H18E)=Sof(H18F)=
 Sof(C19A)=Sof(H19D)=Sof(H19E)=Sof(H19F)=Sof(C20A)=Sof(H20D)=Sof(H20E)=
 Sof(H20F)=Sof(C21A)=Sof(H21C)=Sof(H21D)=Sof(C22A)=Sof(H22C)=Sof(H22D)=
 Sof(C23A)=Sof(H23D)=Sof(H23E)=Sof(H23F)=Sof(C24A)=Sof(H24D)=Sof(H24E)=
 Sof(H24F)=Sof(C25A)=Sof(H25D)=Sof(H25E)=Sof(H25F)=Sof(C26A)=Sof(H26D)=
 Sof(H26E)=Sof(H26F)=Sof(C27A)=Sof(H27C)=Sof(H27D)=Sof(C28A)=Sof(H28C)=
 Sof(H28D)=Sof(C29A)=Sof(H29D)=Sof(H29E)=Sof(H29F)=Sof(C30A)=Sof(H30D)=
 Sof(H30E)=Sof(H30F)=1-FVAR(1)
 Sof(H)=Sof(P1)=Sof(P2)=Sof(P3)=Sof(P4)=Sof(P5)=Sof(P6)=Sof(P7)=Sof(P8)=
 Sof(P9)=Sof(P10)=Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=Sof(C2)=Sof(H2A)=Sof(H2B)=
 Sof(H2C)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(C5)=Sof(H5A)=
 Sof(H5B)=Sof(H5C)=Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(H6C)=Sof(C7)=Sof(H7A)=Sof(H7B)=
 Sof(H7C)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(C10)=
 Sof(H10A)=Sof(H10B)=Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(H11C)=Sof(C12)=Sof(H12A)=
 Sof(H12B)=Sof(H12C)=Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(H13C)=Sof(C14)=Sof(H14A)=
 Sof(H14B)=Sof(H14C)=Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(C16)=Sof(H16A)=Sof(H16B)=
 Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(H18C)=
 Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(H19C)=Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H20C)=
 Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(C23)=Sof(H23A)=
 Sof(H23B)=Sof(H23C)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=Sof(C25)=Sof(H25A)=
 Sof(H25B)=Sof(H25C)=Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(H26C)=Sof(C27)=Sof(H27A)=
 Sof(H27B)=Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(H29C)=
 Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(H30C)=FVAR(1)
 Fixed Uiso: H(0.03)
7.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C9(H9A,H9B), C10(H10A,H10B), C15(H15A,H15B),
 C16(H16A,H16B), C21(H21A,H21B), C22(H22A,H22B), C27(H27A,H27B), C28(H28A,H28B),
  C3A(H3AA,H3AB), C4A(H4AA,H4AB), C9A(H9AA,H9AB), C10A(H10C,H10D), C15A(H15C,
 H15D), C16A(H16C,H16D), C21A(H21C,H21D), C22A(H22C,H22D), C27A(H27C,H27D),
 C28A(H28C,H28D)
7.b Me refined with riding coordinates:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,
 H7B,H7C), C8(H8A,H8B,H8C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,
 H13B,H13C), C14(H14A,H14B,H14C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C),
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C29(H29A,H29B,H29C), C30(H30A,
 H30B,H30C), C1A(H1AA,H1AB,H1AC), C2A(H2AA,H2AB,H2AC), C5A(H5AA,H5AB,H5AC),
 C6A(H6AA,H6AB,H6AC), C7A(H7AA,H7AB,H7AC), C8A(H8AA,H8AB,H8AC), C11A(H11D,H11E,
 H11F), C12A(H12D,H12E,H12F), C13A(H13D,H13E,H13F), C14A(H14D,H14E,H14F),
 C17A(H17D,H17E,H17F), C18A(H18D,H18E,H18F), C19A(H19D,H19E,H19F), C20A(H20D,
 H20E,H20F), C23A(H23D,H23E,H23F), C24A(H24D,H24E,H24F), C25A(H25D,H25E,H25F),
 C26A(H26D,H26E,H26F), C29A(H29D,H29E,H29F), C30A(H30D,H30E,H30F)
;
_shelx_res_checksum              37529
_olex2_submission_special_instructions 'No special instructions were received'