Blue Alkali Dinitrosomethanides: Synthesis, Structure, and Bonding
Harald Brand; Peter Mayer; Kurt Polborn; Axel Schulz; Jan J. Weigand; Journal of the American Chemical Society 127 (2005) 1360–1361; doi:10.1021/ja042877u

data_4111404
_publ_contact_author_address
;
Department Chemie und Biochemie
Ludwig-Maximilians Universit\"at
Butenandtstra\&se 5-13 (Haus F)
D-81377 M\"unchen
Bundesrepublik Deutschland
;
_publ_contact_author_email       lex@cup.uni-muenchen.de
_publ_contact_author_fax         +49-89-2180-77492
_publ_contact_author_name        'Axel Schulz'
_publ_section_title
;
 Blue Alkali Dinitrosomethanides: Synthesis, Structure, and Bonding
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1360
_journal_page_last               1361
_journal_paper_doi               10.1021/ja042877u
_journal_volume                  127
_journal_year                    2005
_chemical_formula_moiety         'Cs, C H N2 O2'
_chemical_formula_sum            'C H Cs N2 O2'
_chemical_formula_weight         205.936
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_author_name               'Mayer, P.'
_audit_block_code                Cs_CHNO_in157_schulz
_audit_creation_date             03-Apr-04
_audit_creation_method           'form98_non/compatible with shelxl97-2'
_audit_update_record             08-Nov-04
_cell_angle_alpha                90.0000
_cell_angle_beta                 99.2655(12)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   4.69210(10)
_cell_length_b                   12.71440(29)
_cell_length_c                   7.84900(20)
_cell_measurement_reflns_used    4060
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      3.134
_cell_volume                     462.140(19)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_refinement
'SHELXL-97 (G. M. Sheldrick. University of G\"ottingen, 97-2 version)'
_computing_structure_solution
;
A. Altomare, M. C. Burla, M. Camalli, G. L. Cascarano, C. Giacovazzo, A.
Guagliardi, A. G. G. Moliterni, G. Polidori, R. Spagna: SIR97: a new tool for
crystal structure determination and refinement; J. Appl. Crystallogr. 1999,
32, 115-119.
;
_diffrn_ambient_temperature      200
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.1352286
_diffrn_orient_matrix_UB_12      0.0354712
_diffrn_orient_matrix_UB_13      0.0940400
_diffrn_orient_matrix_UB_21      -0.0824852
_diffrn_orient_matrix_UB_22      -0.0419693
_diffrn_orient_matrix_UB_23      0.0881941
_diffrn_orient_matrix_UB_31      0.1467658
_diffrn_orient_matrix_UB_32      -0.0562703
_diffrn_orient_matrix_UB_33      -0.0064997
_diffrn_radiation_collimation    0.35
_diffrn_radiation_monochromator  'vertically mounted graphite crystal'
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0470
_diffrn_reflns_av_sigmaI/netI    0.0284
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            7663
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         3.20
_diffrn_source_current           90.00
_diffrn_source_power             4.050
_diffrn_source_type              'FR 591 generator'
_diffrn_source_voltage           45.00
_exptl_absorpt_coefficient_mu    7.873
_exptl_absorpt_correction_T_max  0.8549
_exptl_absorpt_correction_T_min  0.6106
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
'Absorption correction with XRed, rev 1.09, STOE (Darmstadt, Germany)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.95988(12)
_exptl_crystal_description       block
_exptl_crystal_F_000             368
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.421
_refine_diff_density_min         -0.621
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.187
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     59
_refine_ls_number_reflns         1060
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.187
_refine_ls_R_factor_all          0.0231
_refine_ls_R_factor_gt           0.0184
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0019P)^2^+0.1729P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0373
_refine_ls_wR_factor_ref         0.0386
_reflns_number_gt                943
_reflns_number_total             1060
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja042877usi20041125_081745.cif
_cod_data_source_block           in157
_cod_original_cell_volume        462.140(18)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4111404