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_7704762
_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         'C12 H36 B Mn P4'
_chemical_formula_sum            'C12 H36 B Mn P4'
_chemical_formula_weight         370.04
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.8683(5)
_cell_length_b                   11.8704(5)
_cell_length_c                   28.4192(14)
_cell_measurement_reflns_used    9964
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.87
_cell_measurement_theta_min      2.82
_cell_volume                     4003.7(3)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0507
_diffrn_reflns_av_unetI/netI     0.0424
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            35368
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.489
_diffrn_reflns_theta_min         1.716
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.965
_exptl_absorpt_correction_T_max  0.9938
_exptl_absorpt_correction_T_min  0.7091
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 'SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.0730 before and 0.0645 after correction.
The Ratio of minimum to maximum transmission is 0.7135.
The \l/2 correction factor is 0.00150.'
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.228
_exptl_crystal_description       block
_exptl_crystal_F_000             1584
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.383
_exptl_crystal_size_min          0.144
_refine_diff_density_max         1.295
_refine_diff_density_min         -0.565
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.201
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     184
_refine_ls_number_reflns         6389
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.201
_refine_ls_R_factor_all          0.0596
_refine_ls_R_factor_gt           0.0557
_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^)+(0.0265P)^2^+9.4816P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1282
_refine_ls_wR_factor_ref         0.1299
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5994
_reflns_number_total             6389
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01726d3.cif
_cod_data_source_block           MnBH4
_cod_depositor_comments
'Adding full bibliography for 7704762--7704768.cif.'
_cod_database_code               7704762
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.874
_shelx_estimated_absorpt_t_min   0.660
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5075(13)
 0.4925(13)
2. Fixed Uiso
 At 1.2 times of:
  All B(H,H,H,H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 B1-H1 \\sim B1-H2
 with sigma of 0.02
 Mn1-H1 \\sim Mn1-H2
 with sigma of 0.02
4.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C9(H9A,H9B), C10(H10A,H10B)
4.b Idealised Me refined as rotating group:
 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)
;
_shelx_res_checksum              32458
_olex2_submission_special_instructions 'No special instructions were received'