Towards hydrogen-rich ionic (NH4)(BH3NH2BH2NH2BH3) and related molecular NH3BH2NH2BH2NH2BH3
Owarzany, Rafał; Jaroń, Tomasz; Kazimierczuk, Krzysztof; Malinowski, Przemysław J.; Grochala, Wojciech; Fijalkowski, Karol J.; Dalton Transactions  (2023) –; doi:10.1039/D2DT03674F

data_7712200
_publ_section_title
;
 Towards hydrogen-rich ionic (NH4)(BH3NH2BH2NH2BH3) and related molecular
 NH3BH2NH2BH2NH2BH3
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT03674F
_journal_year                    2023
_chemical_formula_sum            'C42 H60 B N4 P'
_chemical_formula_weight         662.72
_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
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                61.751(2)
_cell_angle_beta                 73.618(2)
_cell_angle_gamma                89.605(2)
_cell_formula_units_Z            4
_cell_length_a                   11.7376(3)
_cell_length_b                   19.5388(5)
_cell_length_c                   20.5479(4)
_cell_measurement_reflns_used    24467
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      75.2030
_cell_measurement_theta_min      4.3510
_cell_volume                     3937.71(19)
_computing_cell_refinement       'CrysAlisPro 1.171.40.55a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.55a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.55a (Rigaku OD, 2019)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Atlas'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0602
_diffrn_reflns_av_unetI/netI     0.0385
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            73885
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.815
_diffrn_reflns_theta_min         2.573
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.856
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.690
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.55a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.118
_exptl_crystal_description       block
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.060
_refine_diff_density_max         1.164
_refine_diff_density_min         -0.327
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     905
_refine_ls_number_reflns         16062
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0880
_refine_ls_R_factor_gt           0.0695
_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^)+(0.1120P)^2^+1.4081P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1907
_refine_ls_wR_factor_ref         0.2094
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12195
_reflns_number_total             16062
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03674f3.cif
_cod_data_source_block           exp_1917_a
_cod_original_cell_volume        3937.71(18)
_cod_database_code               7712200
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.847
_shelx_estimated_absorpt_t_max   0.950
_shelx_res_checksum              39276
_shelx_hkl_checksum              63651