#------------------------------------------------------------------------------
#$Date: 2017-01-14 04:17:32 +0200 (Sat, 14 Jan 2017) $
#$Revision: 190486 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/20/2242021.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_2242021
loop_
_publ_author_name
'Grassl, Tobias'
'Korber, Nikolaus'
_publ_section_title
;
 Crystal structure of rubidium methyldiazotate
;
_journal_coeditor_code           PK2593
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              159
_journal_page_last               161
_journal_paper_doi               10.1107/S2056989016020429
_journal_volume                  73
_journal_year                    2017
_chemical_formula_iupac          'Rb +, C H3 N2 O -'
_chemical_formula_moiety         'Rb +, C H3 N2 O -'
_chemical_formula_sum            'C H3 N2 O Rb'
_chemical_formula_weight         144.52
_chemical_name_common            'Rubidium methyldiazotate'
_chemical_name_systematic        'Rubidium methyldiazotate'
_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   difmap
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 114.219(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.86580(10)
_cell_length_b                   8.76140(10)
_cell_length_c                   7.24470(10)
_cell_measurement_reflns_used    8481
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      32.0517
_cell_measurement_theta_min      3.0770
_cell_volume                     397.441(11)
_computing_cell_refinement
;
CrysAlis PRO (Agilent, 2012)
;
_computing_data_collection
;
CrysAlis PRO (Agilent, 2012)
;
_computing_data_reduction
;
CrysAlis PRO (Agilent, 2012)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg & Putz, 2012)
;
_computing_publication_material
;
OLEX2 (Dolomanov et al.,  2009)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
olex2.solve (Bourhis et al.,  2015)
;
_diffrn_ambient_temperature      123.15
_diffrn_detector_area_resol_mean 15.9702
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type
'Agilent SuperNova Dual Source diffractometer with an Eos detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0513
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            13443
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.506
_diffrn_reflns_theta_min         3.444
_exptl_absorpt_coefficient_mu    12.264
_exptl_absorpt_correction_T_max  0.267
_exptl_absorpt_correction_T_min  0.267
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
[CrysAlis PRO (Agilent, 2012) based on expressions derived by
Clark & Reid (1995)]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.415
_exptl_crystal_description       Block
_exptl_crystal_F_000             272
_exptl_crystal_size_max          0.2864
_exptl_crystal_size_mid          0.1741
_exptl_crystal_size_min          0.1507
_refine_diff_density_max         0.562
_refine_diff_density_min         -0.863
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     58
_refine_ls_number_reflns         1210
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0206
_refine_ls_R_factor_gt           0.0173
_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/[σ²(Fo²)+(0.0256P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0412
_refine_ls_wR_factor_ref         0.0416
_reflns_number_gt                1068
_reflns_number_total             1210
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            pk2593sup1.cif
_cod_data_source_block           I
_cod_database_code               2242021
_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+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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
Rb Rb1 0.24027(2) 0.64932(2) 0.44893(2) 0.01283(6) Uani d 1
O O1 0.6929(2) 0.68315(14) 0.5959(2) 0.0159(2) Uani d 1
N N1 0.7933(2) 0.67488(17) 0.4770(2) 0.0163(3) Uani d 1
N N2 0.8203(2) 0.79640(17) 0.3938(2) 0.0159(3) Uani d 1
C C1 0.7331(3) 0.9368(2) 0.4396(3) 0.0194(3) Uani d 1
H H2 0.583(3) 0.928(2) 0.408(4) 0.027(6) Uiso d 1
H H3 0.753(3) 1.018(2) 0.352(3) 0.016(5) Uiso d 1
H H1 0.812(4) 0.967(3) 0.587(5) 0.049(9) Uiso d 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rb Rb -0.9393 2.9676 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-9 -4 4 0.1396
0 -11 -4 0.0844
9 -2 -6 0.1253
0 11 4 0.0897
-6 8 6 0.0904
8 7 -2 0.1195
0 6 -8 0.0625
0 -3 9 0.0746
5 -4 5 0.0954
-5 4 -5 0.0855
1 -10 5 0.0982
1 0 9 0.0726
0 8 -7 0.0624
-1 -4 -8 0.0939
0 -11 4 0.0947
5 -10 0 0.1115
7 -1 -9 0.1032
-8 -5 8 0.1432
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
Rb1 Rb1 Rb1 3_666 2 113.582(6)
Rb1 Rb1 Rb1 4_676 2 85.861(5)
Rb1 Rb1 Rb1 4_676 3_666 77.186(4)
C1 Rb1 Rb1 4_575 3_666 73.60(3)
C1 Rb1 Rb1 4_575 2 67.80(3)
C1 Rb1 Rb1 4_575 4_676 127.36(3)
Rb1 O1 Rb1 4_676 3_666 129.33(5)
N1 O1 Rb1 . 3_666 74.24(8)
N1 O1 Rb1 . 4_676 136.30(10)
Rb1 N1 Rb1 3_666 1_655 95.44(4)
O1 N1 Rb1 . 1_655 146.43(12)
O1 N1 Rb1 . 3_666 80.21(8)
N2 N1 Rb1 . 1_655 72.28(9)
N2 N1 Rb1 . 3_666 159.82(11)
N2 N1 O1 . . 118.93(13)
Rb1 N2 Rb1 1_655 4_675 87.43(4)
N1 N2 Rb1 . 1_655 84.13(10)
N1 N2 Rb1 . 4_675 128.81(11)
N1 N2 C1 . . 116.27(13)
C1 N2 Rb1 . 1_655 141.49(11)
C1 N2 Rb1 . 4_675 101.15(10)
Rb1 C1 Rb1 3_676 4_676 90.16(4)
Rb1 C1 Rb1 4_675 4_676 156.42(6)
Rb1 C1 Rb1 4_675 3_676 113.28(5)
Rb1 C1 H2 3_676 . 94.8(13)
Rb1 C1 H2 4_676 . 78.4(15)
Rb1 C1 H2 4_675 . 101.1(15)
Rb1 C1 H3 4_675 . 58.0(12)
Rb1 C1 H3 3_676 . 55.4(12)
Rb1 C1 H3 4_676 . 144.9(12)
Rb1 C1 H1 3_676 . 63.8(16)
Rb1 C1 H1 4_676 . 39.6(15)
Rb1 C1 H1 4_675 . 149.8(14)
N2 C1 Rb1 . 3_676 152.09(11)
N2 C1 Rb1 . 4_676 102.26(10)
N2 C1 Rb1 . 4_675 55.69(8)
N2 C1 H2 . . 112.1(13)
N2 C1 H3 . . 106.3(11)
N2 C1 H1 . . 111.5(16)
H2 C1 H3 . . 108.5(17)
H2 C1 H1 . . 109(2)
H3 C1 H1 . . 109.3(19)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Rb1 Rb1 4_676 4.22095(16)
Rb1 Rb1 3_666 4.2365(3)
Rb1 Rb1 2 5.27567(17)
Rb1 C1 4_575 3.7471(18)
O1 Rb1 4_676 2.8496(12)
O1 Rb1 3_666 2.9871(12)
O1 N1 . 1.3074(19)
N1 Rb1 1_655 3.1656(15)
N1 Rb1 3_666 2.9173(15)
N1 N2 . 1.274(2)
N2 Rb1 1_655 3.0313(14)
N2 Rb1 4_675 3.0761(15)
N2 C1 . 1.465(2)
C1 Rb1 4_676 3.7471(18)
C1 Rb1 4_675 3.6538(18)
C1 Rb1 3_676 3.7031(19)
C1 H2 . 0.97(2)
C1 H3 . 1.00(2)
C1 H1 . 1.02(3)

_cod_database_fobs_code 2242021
