#------------------------------------------------------------------------------
#$Date: 2020-08-06 15:50:34 +0200 (jue 06 de ago de 2020) $
#$Revision: 254945 $
#$URL: svn://www.crystallography.net/cod/cif/7/70/47/7704766.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7704766
loop_
_publ_author_name
'Price, Jeffrey S.'
'DeJordy, Declan M.'
'Emslie, David J. H.'
'Britten, James F.'
_publ_section_title
;
 Reactions of [(dmpe)₂MnH(C₂H₄)]:
 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         'C15 H42 Mn P5'
_chemical_formula_sum            'C15 H42 Mn P5'
_chemical_formula_weight         432.27
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-04-06
_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                91.032(3)
_cell_angle_beta                 106.889(3)
_cell_angle_gamma                113.056(3)
_cell_formula_units_Z            2
_cell_length_a                   9.2251(10)
_cell_length_b                   9.4251(10)
_cell_length_c                   15.1932(16)
_cell_measurement_reflns_used    2093
_cell_measurement_temperature    100
_cell_measurement_theta_max      23.1915
_cell_measurement_theta_min      2.3865
_cell_volume                     1150.0(2)
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1174
_diffrn_reflns_av_unetI/netI     0.1203
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            19746
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.309
_diffrn_reflns_theta_min         1.417
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.916
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6094
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.0695 before and 0.0560 after correction.
The Ratio of minimum to maximum transmission is 0.8175.
The λ/2 correction factor is 0.00150.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.248
_exptl_crystal_description       Block
_exptl_crystal_F_000             464
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   0.7454
_exptl_transmission_factor_min   0.6094
_refine_diff_density_max         0.851
_refine_diff_density_min         -0.747
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     205
_refine_ls_number_reflns         4659
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.1237
_refine_ls_R_factor_gt           0.0674
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0450P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1023
_refine_ls_wR_factor_ref         0.1159
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3014
_reflns_number_total             4659
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0dt01726d3.cif
_cod_data_source_block           MnHPMe3_trans
_cod_depositor_comments
'Adding full bibliography for 7704762--7704768.cif.'
_cod_database_code               7704766
_shelx_shelxl_version_number     2016/6
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.991
_shelx_estimated_absorpt_t_min   0.982
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B), C12(H12A,H12B), C13(H13A,H13B)
2.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,
 H5B,H5C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,
 H11C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C)
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.58530(8) 0.69080(7) 0.73545(4) 0.01133(18) Uani 1 1 d . . . . .
H1 H 0.568(6) 0.591(6) 0.664(4) 0.069(18) Uiso 1 1 d . . . . .
P1 P 0.61640(15) 0.85573(13) 0.85398(8) 0.0170(3) Uani 1 1 d . . . . .
P2 P 0.77135(15) 0.60543(13) 0.81248(9) 0.0203(3) Uani 1 1 d . . . . .
P3 P 0.79399(14) 0.84351(13) 0.68927(8) 0.0171(3) Uani 1 1 d . . . . .
P4 P 0.39728(14) 0.74496(12) 0.62980(8) 0.0143(3) Uani 1 1 d . . . . .
P5 P 0.37009(14) 0.48010(13) 0.74091(8) 0.0168(3) Uani 1 1 d . . . . .
C1 C 0.7398(6) 1.0691(5) 0.8647(3) 0.0324(13) Uani 1 1 d . . . . .
H1A H 0.851772 1.088880 0.868087 0.049 Uiso 1 1 calc GR . . . .
H1B H 0.741162 1.120912 0.920086 0.049 Uiso 1 1 calc GR . . . .
H1C H 0.690335 1.107680 0.811432 0.049 Uiso 1 1 calc GR . . . .
C2 C 0.4304(6) 0.8690(6) 0.8721(4) 0.0363(14) Uani 1 1 d . . . . .
H2A H 0.355874 0.870968 0.813453 0.055 Uiso 1 1 calc GR . . . .
H2B H 0.465049 0.962615 0.913631 0.055 Uiso 1 1 calc GR . . . .
H2C H 0.374586 0.780126 0.898477 0.055 Uiso 1 1 calc GR . . . .
C3 C 0.7112(6) 0.8402(6) 0.9778(3) 0.0329(13) Uani 1 1 d . . . . .
H3A H 0.644209 0.741975 0.992008 0.049 Uiso 1 1 calc GR . . . .
H3B H 0.716848 0.923605 1.017741 0.049 Uiso 1 1 calc GR . . . .
H3C H 0.821428 0.846904 0.987443 0.049 Uiso 1 1 calc GR . . . .
C4 C 0.8104(6) 0.4611(6) 0.7484(3) 0.0321(13) Uani 1 1 d . . . . .
H4A H 0.711917 0.365197 0.728167 0.048 Uiso 1 1 calc GR . . . .
H4B H 0.900582 0.442294 0.788642 0.048 Uiso 1 1 calc GR . . . .
H4C H 0.838881 0.501453 0.695209 0.048 Uiso 1 1 calc GR . . . .
C5 C 0.7781(7) 0.5170(6) 0.9194(3) 0.0335(13) Uani 1 1 d . . . . .
H5A H 0.789756 0.590271 0.968492 0.050 Uiso 1 1 calc GR . . . .
H5B H 0.871120 0.489208 0.936723 0.050 Uiso 1 1 calc GR . . . .
H5C H 0.676875 0.425162 0.908919 0.050 Uiso 1 1 calc GR . . . .
C6 C 0.9856(6) 0.7684(6) 0.8493(4) 0.0393(14) Uani 1 1 d . . . . .
H6A H 1.007250 0.824881 0.909093 0.047 Uiso 1 1 calc R . . . .
H6B H 1.067417 0.725303 0.856598 0.047 Uiso 1 1 calc R . . . .
C7 C 1.0039(6) 0.8846(5) 0.7757(3) 0.0286(12) Uani 1 1 d . . . . .
H7A H 1.076088 0.873071 0.743340 0.034 Uiso 1 1 calc R . . . .
H7B H 1.054342 0.991067 0.807205 0.034 Uiso 1 1 calc R . . . .
C8 C 0.8314(6) 1.0411(5) 0.6567(3) 0.0311(12) Uani 1 1 d . . . . .
H8A H 0.739664 1.034357 0.604170 0.047 Uiso 1 1 calc GR . . . .
H8B H 0.932157 1.081890 0.640948 0.047 Uiso 1 1 calc GR . . . .
H8C H 0.841789 1.108930 0.708244 0.047 Uiso 1 1 calc GR . . . .
C9 C 0.8190(6) 0.7651(5) 0.5843(3) 0.0291(12) Uani 1 1 d . . . . .
H9A H 0.827045 0.667431 0.592963 0.044 Uiso 1 1 calc GR . . . .
H9B H 0.918436 0.837799 0.574712 0.044 Uiso 1 1 calc GR . . . .
H9C H 0.724510 0.749415 0.531084 0.044 Uiso 1 1 calc GR . . . .
C10 C 0.3735(6) 0.7057(5) 0.5056(3) 0.0223(11) Uani 1 1 d . . . . .
H10A H 0.466469 0.782756 0.492296 0.034 Uiso 1 1 calc GR . . . .
H10B H 0.272330 0.709901 0.467760 0.034 Uiso 1 1 calc GR . . . .
H10C H 0.369462 0.604001 0.492205 0.034 Uiso 1 1 calc GR . . . .
C11 C 0.3792(6) 0.9348(5) 0.6270(3) 0.0245(11) Uani 1 1 d . . . . .
H11A H 0.370203 0.966113 0.684920 0.037 Uiso 1 1 calc GR . . . .
H11B H 0.281908 0.923780 0.576986 0.037 Uiso 1 1 calc GR . . . .
H11C H 0.476225 1.012362 0.617563 0.037 Uiso 1 1 calc GR . . . .
C12 C 0.1817(5) 0.6169(5) 0.6276(3) 0.0183(10) Uani 1 1 d . . . . .
H12A H 0.153843 0.659773 0.675651 0.022 Uiso 1 1 calc R . . . .
H12B H 0.101752 0.609034 0.567786 0.022 Uiso 1 1 calc R . . . .
C13 C 0.1776(5) 0.4554(5) 0.6448(3) 0.0204(11) Uani 1 1 d . . . . .
H13A H 0.171764 0.400060 0.588569 0.025 Uiso 1 1 calc R . . . .
H13B H 0.079875 0.394739 0.661712 0.025 Uiso 1 1 calc R . . . .
C14 C 0.2858(6) 0.4468(6) 0.8399(3) 0.0325(13) Uani 1 1 d . . . . .
H14A H 0.373079 0.456776 0.895963 0.049 Uiso 1 1 calc GR . . . .
H14B H 0.198048 0.343858 0.827646 0.049 Uiso 1 1 calc GR . . . .
H14C H 0.242874 0.522449 0.847117 0.049 Uiso 1 1 calc GR . . . .
C15 C 0.3649(6) 0.2838(5) 0.7184(4) 0.0314(13) Uani 1 1 d . . . . .
H15A H 0.394078 0.275762 0.663430 0.047 Uiso 1 1 calc GR . . . .
H15B H 0.254875 0.205839 0.709750 0.047 Uiso 1 1 calc GR . . . .
H15C H 0.442899 0.268255 0.770501 0.047 Uiso 1 1 calc GR . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
P1 Mn1 H1 180(2) . . ?
P2 Mn1 H1 83(2) . . ?
P2 Mn1 P1 97.05(5) . . ?
P2 Mn1 P3 82.77(5) . . ?
P2 Mn1 P4 166.76(5) . . ?
P3 Mn1 H1 81(2) . . ?
P3 Mn1 P1 99.09(5) . . ?
P3 Mn1 P4 93.41(5) . . ?
P4 Mn1 H1 84(2) . . ?
P4 Mn1 P1 96.08(5) . . ?
P5 Mn1 H1 79(2) . . ?
P5 Mn1 P1 101.44(5) . . ?
P5 Mn1 P2 93.82(5) . . ?
P5 Mn1 P3 159.45(5) . . ?
P5 Mn1 P4 85.32(5) . . ?
C1 P1 Mn1 121.14(16) . . ?
C1 P1 C2 96.3(2) . . ?
C1 P1 C3 95.8(2) . . ?
C2 P1 Mn1 120.12(17) . . ?
C2 P1 C3 94.6(2) . . ?
C3 P1 Mn1 122.39(16) . . ?
C4 P2 Mn1 118.64(16) . . ?
C4 P2 C6 99.0(2) . . ?
C5 P2 Mn1 127.37(17) . . ?
C5 P2 C4 96.8(2) . . ?
C5 P2 C6 100.4(2) . . ?
C6 P2 Mn1 110.04(17) . . ?
C7 P3 Mn1 112.72(16) . . ?
C8 P3 Mn1 126.89(16) . . ?
C8 P3 C7 100.2(2) . . ?
C9 P3 Mn1 117.42(16) . . ?
C9 P3 C7 99.4(2) . . ?
C9 P3 C8 95.6(2) . . ?
C10 P4 Mn1 118.55(15) . . ?
C10 P4 C11 97.5(2) . . ?
C10 P4 C12 99.7(2) . . ?
C11 P4 Mn1 126.67(16) . . ?
C11 P4 C12 98.9(2) . . ?
C12 P4 Mn1 110.94(14) . . ?
C13 P5 Mn1 110.56(14) . . ?
C14 P5 Mn1 125.30(17) . . ?
C14 P5 C13 99.7(2) . . ?
C15 P5 Mn1 120.10(16) . . ?
C15 P5 C13 98.7(2) . . ?
C15 P5 C14 97.8(2) . . ?
P1 C1 H1A 109.5 . . ?
P1 C1 H1B 109.5 . . ?
P1 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
P1 C2 H2A 109.5 . . ?
P1 C2 H2B 109.5 . . ?
P1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
P1 C3 H3A 109.5 . . ?
P1 C3 H3B 109.5 . . ?
P1 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
P2 C4 H4A 109.5 . . ?
P2 C4 H4B 109.5 . . ?
P2 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
P2 C5 H5A 109.5 . . ?
P2 C5 H5B 109.5 . . ?
P2 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
P2 C6 H6A 109.4 . . ?
P2 C6 H6B 109.4 . . ?
H6A C6 H6B 108.0 . . ?
C7 C6 P2 111.3(3) . . ?
C7 C6 H6A 109.4 . . ?
C7 C6 H6B 109.4 . . ?
P3 C7 H7A 109.6 . . ?
P3 C7 H7B 109.6 . . ?
C6 C7 P3 110.2(3) . . ?
C6 C7 H7A 109.6 . . ?
C6 C7 H7B 109.6 . . ?
H7A C7 H7B 108.1 . . ?
P3 C8 H8A 109.5 . . ?
P3 C8 H8B 109.5 . . ?
P3 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
P3 C9 H9A 109.5 . . ?
P3 C9 H9B 109.5 . . ?
P3 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
P4 C10 H10A 109.5 . . ?
P4 C10 H10B 109.5 . . ?
P4 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
P4 C11 H11A 109.5 . . ?
P4 C11 H11B 109.5 . . ?
P4 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
P4 C12 H12A 110.2 . . ?
P4 C12 H12B 110.2 . . ?
H12A C12 H12B 108.5 . . ?
C13 C12 P4 107.3(3) . . ?
C13 C12 H12A 110.2 . . ?
C13 C12 H12B 110.2 . . ?
P5 C13 H13A 109.9 . . ?
P5 C13 H13B 109.9 . . ?
C12 C13 P5 109.1(3) . . ?
C12 C13 H13A 109.9 . . ?
C12 C13 H13B 109.9 . . ?
H13A C13 H13B 108.3 . . ?
P5 C14 H14A 109.5 . . ?
P5 C14 H14B 109.5 . . ?
P5 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
P5 C15 H15A 109.5 . . ?
P5 C15 H15B 109.5 . . ?
P5 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mn1 H1 1.36(5) . ?
Mn1 P1 2.2343(13) . ?
Mn1 P2 2.2161(14) . ?
Mn1 P3 2.2183(13) . ?
Mn1 P4 2.2250(13) . ?
Mn1 P5 2.2148(13) . ?
P1 C1 1.858(5) . ?
P1 C2 1.864(5) . ?
P1 C3 1.866(4) . ?
P2 C4 1.863(5) . ?
P2 C5 1.835(5) . ?
P2 C6 1.878(5) . ?
P3 C7 1.882(5) . ?
P3 C8 1.860(4) . ?
P3 C9 1.857(5) . ?
P4 C10 1.849(4) . ?
P4 C11 1.861(4) . ?
P4 C12 1.869(4) . ?
P5 C13 1.870(4) . ?
P5 C14 1.863(5) . ?
P5 C15 1.854(4) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 C7 1.578(7) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C12 C13 1.537(6) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
