Salts of 1-(chloromethyl)-1,1-dimethylhydrazine and ionic liquids
Miró Sabaté, Carles; Delalu, Henri; Forquet, Valérian; Jeanneau, Erwann; RSC Advances 2 (2012) 3691–; doi:10.1039/c2ra00968d

data_7238574
_publ_section_title
;
 Salts of 1-(chloromethyl)-1,1-dimethylhydrazine and ionic liquids
;
_journal_issue                   9
_journal_name_full               'RSC Advances'
_journal_page_first              3691
_journal_paper_doi               10.1039/c2ra00968d
_journal_volume                  2
_journal_year                    2012
_chemical_formula_moiety         'C12 H14 Ba N6 O19, H2 O'
_chemical_formula_sum            'C12 H16 Ba N6 O20'
_chemical_formula_weight         701.63
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                84.647(5)
_cell_angle_beta                 80.070(6)
_cell_angle_gamma                86.803(6)
_cell_formula_units_Z            2
_cell_length_a                   6.6417(5)
_cell_length_b                   11.5885(8)
_cell_length_c                   15.0331(9)
_cell_measurement_reflns_used    11802
_cell_measurement_temperature    110
_cell_measurement_theta_max      29.5057
_cell_measurement_theta_min      3.3961
_cell_volume                     1133.82(14)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET)
(compiled Nov 25 2010,17:55:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET)
(compiled Nov 25 2010,17:55:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET)
(compiled Nov 25 2010,17:55:46)
;
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      110
_diffrn_detector_area_resol_mean 10.4685
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.909
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.066
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            28809
_diffrn_reflns_theta_full        26.908
_diffrn_reflns_theta_max         29.569
_diffrn_reflns_theta_min         3.403
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.864
_exptl_absorpt_correction_T_max  0.869
_exptl_absorpt_correction_T_min  0.587
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET)
(compiled Nov 25 2010,17:55:46)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.055
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             692
_exptl_crystal_size_max          0.509
_exptl_crystal_size_mid          0.105
_exptl_crystal_size_min          0.089
_refine_diff_density_max         0.99
_refine_diff_density_min         -1.80
_refine_ls_extinction_coef       22(3)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   0.9995
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     353
_refine_ls_number_reflns         5785
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0398
_refine_ls_R_factor_gt           0.0358
_refine_ls_shift/su_max          0.0006222
_refine_ls_shift/su_mean         0.0000130
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
0.137E+04 0.204E+04 0.109E+04 299.
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0773
_refine_ls_wR_factor_gt          0.0693
_refine_ls_wR_factor_ref         0.0773
_reflns_limit_h_max              9
_reflns_limit_h_min              -8
_reflns_limit_k_max              15
_reflns_limit_k_min              -15
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                5298
_reflns_number_total             5785
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0398
_oxford_refine_ls_scale          4.35(5)
_oxford_reflns_number_all        5785
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_cod_data_source_file            c2ra00968d.txt
_cod_data_source_block           BaPic_6H2O
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Triclinic' was changed to
'triclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C12 H16 Ba1 N6 O20'
_cod_database_code               7238574
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S
CONT EXTPARAM
RIDE C ( 4,X'S) H ( 41,X'S)
RIDE C ( 6,X'S) H ( 61,X'S)
RIDE C ( 20,X'S) H ( 201,X'S)
RIDE C ( 22,X'S) H ( 221,X'S)
RIDE O ( 33,X'S) H ( 332,X'S) H ( 331,X'S)
RIDE O ( 34,X'S) H ( 342,X'S) H ( 341,X'S)
RIDE O ( 35,X'S) H ( 352,X'S) H ( 351,X'S)
RIDE O ( 36,X'S) H ( 362,X'S) H ( 361,X'S)
RIDE O ( 37,X'S) H ( 372,X'S) H ( 371,X'S)
RIDE O ( 38,X'S) H ( 382,X'S) H ( 381,X'S)
END
;
_iucr_refine_instruction_details_restraints
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NO
REM HREST START (DO NOT REMOVE THIS LINE)
REM HREST END (DO NOT REMOVE THIS LINE)
END
;