#------------------------------------------------------------------------------
#$Date: 2018-03-27 07:57:23 +0300 (Tue, 27 Mar 2018) $
#$Revision: 207125 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/30/06/2300631.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2300631
loop_
_publ_author_name
'Solar, Michael'
'Trapp, Nils'
_publ_section_title
;
 \mCHILL: a lightweight, modular system for handling crystalline samples
 at low temperatures under inert conditions
;
_journal_coeditor_code           GJ5200
_journal_issue                   2
_journal_name_full               'Journal of Applied Crystallography'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S1600576718003291
_journal_volume                  51
_journal_year                    2018
_chemical_formula_moiety         '0.25(B4 H16 Li4)'
_chemical_formula_sum            'B H4 Li'
_chemical_formula_weight         21.78
_chemical_name_systematic        'Lithium borohydride'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     iterative
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.1374(7)
_cell_length_b                   4.4172(5)
_cell_length_c                   6.7029(8)
_cell_measurement_reflns_used    322
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      77.1940
_cell_measurement_theta_min      9.0690
_cell_volume                     211.32(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.31d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.31d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.31d (Rigaku OD, 2017)'
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      100.00(10)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, Pilatus 300K'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0307
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            527
_diffrn_reflns_theta_full        66.020
_diffrn_reflns_theta_max         66.020
_diffrn_reflns_theta_min         9.078
_exptl_absorpt_coefficient_mu    0.094
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55327
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.31d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    0.685
_exptl_crystal_description       plank
_exptl_crystal_F_000             48
_exptl_crystal_size_max          0.125
_exptl_crystal_size_mid          0.082
_exptl_crystal_size_min          0.064
_refine_diff_density_max         0.156
_refine_diff_density_min         -0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.155
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     23
_refine_ls_number_reflns         209
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.155
_refine_ls_R_factor_all          0.0581
_refine_ls_R_factor_gt           0.0560
_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)+(0.1068P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1358
_refine_ls_wR_factor_ref         0.1381
_reflns_number_gt                195
_reflns_number_total             209
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            gj5200sup1.cif
_cod_data_source_block           sm090218_1_1
_cod_original_cell_volume        211.33(4)
_cod_database_code               2300631
_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.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
B B4 0.80450(18) 0.750000 0.57052(18) 0.0250(7) Uani d 1
H H4A 0.7136(13) 0.546(3) 0.5706(15) 0.034(3) Uiso d 1
H H4B 0.899(2) 0.750000 0.436(2) 0.040(4) Uiso d 1
H H4C 0.8911(18) 0.750000 0.709(3) 0.041(4) Uiso d 1
Li Li3 0.6591(3) 0.750000 0.8872(3) 0.0305(8) Uani d 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
B B 0.0090 0.0039 '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'
Li Li 0.0008 0.0003 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
Li3 B4 Li3 . 2_664 118.64(4)
Li3 B4 Li3 2_664 2_674 120.76(9)
Li3 B4 Li3 . 2_674 118.64(4)
Li3 B4 Li3 2_664 6_657 87.26(6)
Li3 B4 Li3 . 6_657 109.66(6)
Li3 B4 Li3 2_674 6_657 87.26(6)
B4 Li3 B4 . 2_675 112.93(5)
B4 Li3 B4 2_675 6_557 92.74(6)
B4 Li3 B4 . 2_665 112.93(5)
B4 Li3 B4 2_665 6_557 92.74(6)
B4 Li3 B4 . 6_557 122.43(10)
B4 Li3 B4 2_675 2_665 120.76(9)
B4 Li3 Li3 . 5_667 132.15(8)
B4 Li3 Li3 2_665 5_667 46.44(4)
B4 Li3 Li3 . 5_677 132.15(8)
B4 Li3 Li3 2_675 5_677 46.44(4)
B4 Li3 Li3 6_557 5_667 46.30(5)
B4 Li3 Li3 6_557 5_677 46.30(5)
B4 Li3 Li3 2_675 5_667 113.88(9)
B4 Li3 Li3 2_665 5_677 113.88(9)
Li3 Li3 Li3 5_667 5_677 77.98(8)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
B4 Li3 . 2.363(2)
B4 Li3 2_674 2.5406(12)
B4 Li3 6_657 2.547(2)
B4 Li3 2_664 2.5406(12)
Li3 Li3 5_667 3.510(3)
Li3 Li3 5_677 3.510(3)

_cod_database_fobs_code 2300631
