Transformation of the ionic liquid [EMIM][B(CN)4] into anionic and neutral lanthanum tetracyanoborate coordination polymers by ionothermal reactions.
Zottnick, Sven H.; Finze, Maik; Müller-Buschbaum, Klaus; Chemical communications (Cambridge, England) 53 (2017) 5193–5195; doi:10.1039/c7cc01378g

data_7119991
_publ_section_title
;
 Transformation of the ionic liquid [EMIM][B(CN)4] into anionic and
 neutral lanthanum tetracyanoborate coordination polymers by ionothermal
 reactions.
;
_journal_issue                   37
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              5193
_journal_page_last               5195
_journal_paper_doi               10.1039/c7cc01378g
_journal_volume                  53
_journal_year                    2017
_chemical_formula_moiety         'C12 H6 B3 La N13 O6, C6 H11 N2'
_chemical_formula_sum            'C18 H17 B3 La N15 O6'
_chemical_formula_weight         710.80
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2017-01-27
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.12 svn.r3133 for OlexSys, GUI svn.r4987)
;
_audit_update_record
;
2017-02-15 deposited with the CCDC.
2017-04-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.85(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.5610(19)
_cell_length_b                   20.688(4)
_cell_length_c                   16.487(3)
_cell_measurement_reflns_used    4059
_cell_measurement_temperature    100
_cell_measurement_theta_max      56.478
_cell_measurement_theta_min      4.691
_cell_volume                     3152.2(11)
_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      100.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0461
_diffrn_reflns_av_unetI/netI     0.0324
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            48007
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.326
_diffrn_reflns_theta_min         1.613
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.412
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6821
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.0685 before and 0.0513 after correction.
The Ratio of minimum to maximum transmission is 0.9147.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.498
_exptl_crystal_description       block
_exptl_crystal_F_000             1400
_exptl_crystal_size_max          0.225
_exptl_crystal_size_mid          0.126
_exptl_crystal_size_min          0.056
_refine_diff_density_max         1.649
_refine_diff_density_min         -1.134
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     414
_refine_ls_number_reflns         7852
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.211
_refine_ls_R_factor_all          0.0392
_refine_ls_R_factor_gt           0.0302
_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^)+(0.0306P)^2^+5.6225P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0704
_refine_ls_wR_factor_ref         0.0746
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6648
_reflns_number_total             7852
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc01378g2.cif
_cod_data_source_block           EMIM_La_NO3_B_CN4_H2O3
_cod_depositor_comments
'Adding full bibliography for 7119990--7119991.cif.'
_cod_original_cell_volume        3152.2(12)
_cod_database_code               7119991
_shelxl_version_number           2014/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C15-C16
 2.5 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B)
3.b Aromatic/amide H refined with riding coordinates:
 C18(H18), C17(H17), C14(H14)
3.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C16(H16A,H16B,H16C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'