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_7704768
_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 H56 B Mn P4'
_chemical_formula_sum            'C30 H56 B Mn P4'
_chemical_formula_weight         606.37
_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     direct
_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                90.611(4)
_cell_angle_beta                 101.870(5)
_cell_angle_gamma                104.056(5)
_cell_formula_units_Z            2
_cell_length_a                   10.068(3)
_cell_length_b                   12.286(3)
_cell_length_c                   13.967(3)
_cell_measurement_reflns_used    9326
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.84
_cell_measurement_theta_min      2.20
_cell_volume                     1636.7(7)
_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      100.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.964
_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_unetI/netI     0.0562
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7863
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.435
_diffrn_reflns_theta_min         1.493
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.617
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.

Final HKLF 4 output contains 55303 reflections, Rint = 0.0528
 (22620 with I > 3sig(I), Rint = 0.0322)
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.230
_exptl_crystal_description       Prism
_exptl_crystal_F_000             652
_exptl_crystal_size_max          0.198
_exptl_crystal_size_mid          0.164
_exptl_crystal_size_min          0.072
_exptl_transmission_factor_max   0.745686
_exptl_transmission_factor_min   0.643564
_refine_diff_density_max         0.554
_refine_diff_density_min         -0.437
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     348
_refine_ls_number_reflns         7863
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0798
_refine_ls_R_factor_gt           0.0468
_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/[\s^2^(Fo^2^)+(0.0355P)^2^+1.5622P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0885
_refine_ls_wR_factor_ref         0.0995
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5865
_reflns_number_total             7863
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01726d3.cif
_cod_data_source_block           MnH_BMes2
_cod_depositor_comments
'Adding full bibliography for 7704762--7704768.cif.'
_cod_database_code               7704768
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.957
_shelx_estimated_absorpt_t_min   0.888
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5778(12)
 0.4222(12)
2. 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
3.a Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C22(H22A,H22B), C27(H27A,H27B), C28(H28A,H28B)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C12(H12), C14(H14)
3.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C16(H16A,H16B,H16C),
 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)
;
_shelx_res_checksum              98431
_olex2_submission_special_instructions 'No special instructions were received'