Borohydride-containing coordination polymers: synthesis, air stability and dehydrogenation
Kadota, Kentaro; Duong, Nghia Tuan; Nishiyama, Yusuke; Sivaniah, Easan; Kitagawa, Susumu; Horike, Satoshi; Chemical Science  (2019) –; doi:10.1039/C9SC00731H

data_1551042
_publ_section_title
;
 Borohydride-containing coordination polymers: synthesis, air stability
 and dehydrogenation
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C9SC00731H
_journal_year                    2019
_chemical_formula_moiety         'C13 H22 B2 N2 Zn'
_chemical_formula_sum            'C13 H22 B2 N2 Zn'
_chemical_formula_weight         293.31
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-06-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-07-13 deposited with the CCDC.    2019-05-13 downloaded from the CCDC.
;
_cell_angle_alpha                91.996(5)
_cell_angle_beta                 90.216(5)
_cell_angle_gamma                94.748(5)
_cell_formula_units_Z            2
_cell_length_a                   5.2876(3)
_cell_length_b                   10.9187(7)
_cell_length_c                   12.7971(7)
_cell_measurement_reflns_used    5948
_cell_measurement_temperature    93
_cell_measurement_theta_max      30.5270
_cell_measurement_theta_min      2.4220
_cell_volume                     735.83(7)
_computing_cell_refinement       'CrysAlisPro 1.171.40.12b (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.12b (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.12b (Rigaku OD, 2018)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      93
_diffrn_detector                 'Rigaku HyPix-6000 area detector'
_diffrn_detector_area_resol_mean 10.0
_diffrn_detector_type            'HPC area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.861
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     11.00  97.00   0.50    5.00    --    8.10  35.00 135.00  172
  2  \w    -62.00 -15.00   0.50    5.00    --    8.10 -35.00 -21.00   94
  3  \w    -41.00  81.00   0.50    5.00    --   -7.30  38.00   0.00  244
  4  \w    -39.00  30.00   0.50    5.00    --   -7.30 -82.00 -60.00  138
  5  \w     17.00  44.00   0.50    5.00    --    8.10  77.00  30.00   54
  6  \w    -18.00  10.00   0.50    5.00    --    8.10  57.00 150.00   56
  7  \w     13.00  45.00   0.50    5.00    --    8.10  57.00 150.00   64
  8  \w    -29.00  48.00   0.50    5.00    --    8.10  77.00 -90.00  154
  9  \w    -27.00  63.00   0.50    5.00    --    8.10  38.00 -60.00  180
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB Synergy-R'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0863802000
_diffrn_orient_matrix_UB_12      -0.0500986000
_diffrn_orient_matrix_UB_13      -0.0167348000
_diffrn_orient_matrix_UB_21      0.1016901000
_diffrn_orient_matrix_UB_22      -0.0302237000
_diffrn_orient_matrix_UB_23      -0.0222552000
_diffrn_orient_matrix_UB_31      0.0180803000
_diffrn_orient_matrix_UB_32      -0.0288151000
_diffrn_orient_matrix_UB_33      0.0479594000
_diffrn_radiation_monochromator  'multi-layer mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0318
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.861
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10420
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.861
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.022
_diffrn_reflns_theta_min         2.415
_diffrn_source                   'rotating anode X-ray generator'
_diffrn_source_type              PhotonJet-R
_exptl_absorpt_coefficient_mu    1.651
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93494
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.12b (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_description       prism
_exptl_crystal_F_000             308
_exptl_crystal_size_max          0.176
_exptl_crystal_size_mid          0.137
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.182
_refine_diff_density_min         -0.502
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         10420
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0553
_refine_ls_R_factor_gt           0.0484
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0793P)^2^+0.3990P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1272
_refine_ls_wR_factor_ref         0.1302
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9208
_reflns_number_total             10420
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc00731h2.cif
_cod_data_source_block           Zn-dpp
_cod_database_code               1551042
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H B N Zn'
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.4933(13)
 0.5067(13)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
3.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C7(H7A,H7B), C6(H6A,H6B)
3.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C9(H9), C13(H13), C10(H10), C2(H2), C1(H1), C4(H4), C12(H12)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.243
_oxdiff_exptl_absorpt_empirical_full_min 0.780
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2
_twin_special_details
;
Component 2 rotated by 179.9356\% 
 around [-0.00 -0.03 1.00] (reciprocal) or [-0.00 0.00 1.00] (direct)
;