Challenges in the synthetic routes to Mn(BH4)2: insight into intermediate compounds.
Tumanov, Nikolay A.; Safin, Damir A.; Richter, Bo; Łodziana, Zbigniew; Jensen, Torben R.; Garcia, Yann; Filinchuk, Yaroslav; Dalton transactions (Cambridge, England : 2003) 44 (2015) 6571–6580; doi:10.1039/c4dt03807j

data_7033962
_publ_section_title
;
 Challenges in the synthetic routes to Mn(BH4)2: insight into intermediate
 compounds.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6571
_journal_page_last               6580
_journal_paper_doi               10.1039/c4dt03807j
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C8 H40 B5 Mn2 Na O2'
_chemical_formula_sum            'C8 H40 B5 Mn2 Na O2'
_chemical_formula_weight         355.32
_chemical_name_common
'sodium dimanganese pentaborohydride bis(diethyl ether)'
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2014-02-06 deposited with the CCDC.
2015-02-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.338(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.5133(6)
_cell_length_b                   7.4487(3)
_cell_length_c                   10.7119(5)
_cell_measurement_reflns_used    1847
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.2524
_cell_measurement_theta_min      3.0661
_cell_volume                     1121.94(9)
_computing_cell_refinement       'CrysAlisPro (Agilent Technologies, 2013)'
_computing_data_reduction        'CrysAlisPro (Agilent Technologies, 2013)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 6.666
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'MAR345 image plate'
_diffrn_measurement_method       '111 images, \D\F 1.5\% '
_diffrn_radiation_monochromator  'Xenocs Fox3D mirror'
_diffrn_radiation_source         'Rigaku UltraX 18 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0390
_diffrn_reflns_av_unetI/netI     0.0462
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4030
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.944
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.045
_diffrn_reflns_theta_min         2.897
_exptl_absorpt_coefficient_mu    1.136
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54282
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.052
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             380
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.565
_refine_diff_density_min         -0.339
_refine_diff_density_rms         0.076
_refine_ls_abs_structure_details
;
 Flack x determined using 722 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.05(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     115
_refine_ls_number_reflns         2093
_refine_ls_number_restraints     59
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0659
_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^)+(0.0959P)^2^+1.2554P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1459
_refine_ls_wR_factor_ref         0.1545
_reflns_Friedel_coverage         0.780
_reflns_Friedel_fraction_full    0.946
_reflns_Friedel_fraction_max     0.899
_reflns_number_gt                1808
_reflns_number_total             2093
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt03807j1.cif
_cod_data_source_block           NaMn2BH4
_cod_depositor_comments
;Adding full bibliography for 7033961--7033963.cif.

The following automatic conversions were performed:

'_atom_sites_solution_secondary' value 'diffmap' was changed to
'difmap'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_cell_volume        1121.96(9)
_cod_database_code               7033962
_shelx_estimated_absorpt_t_min   0.805
_shelx_estimated_absorpt_t_max   0.925
_shelxl_version_number           2014-1
_shelx_res_checksum              58197
_shelx_hkl_checksum              58557