Synthesis and crystal structure of [Cs([2.2.2]crypt)]~2~[Mo(CO)~5~]
Kaas, Marina; Korber, Nikolaus; IUCrData 4 (2019) x191244–; doi:10.1107/S2414314619012446

data_1552332
_publ_section_title
;
 Synthesis and crystal structure of [Cs([2.2.2]crypt)]~2~[Mo(CO)~5~]
;
_journal_coeditor_code           WM4112
_journal_issue                   9
_journal_name_full               IUCrData
_journal_page_first              x191244
_journal_paper_doi               10.1107/S2414314619012446
_journal_volume                  4
_journal_year                    2019
_chemical_formula_iupac          '[Cs (C18 H36 N2 O6)]2 [Mo (C O)5]'
_chemical_formula_moiety         '2(C18 H36 Cs1 N2 O6 +), C5 Mo O5 2-'
_chemical_formula_sum            'C41 H72 Cs2 Mo N4 O17'
_chemical_formula_weight         1254.78
_chemical_name_systematic
;
Bis[(4,7,13,16,21,24-hexaoxa-1,10-diazabicyclo[8.8.8]hexacosane)caesium]
pentacarbonylmolybdate
;
_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   geom
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90.9580(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.22430(10)
_cell_length_b                   16.1431(2)
_cell_length_c                   24.3966(3)
_cell_measurement_reflns_used    16518
_cell_measurement_temperature    122.99(10)
_cell_measurement_theta_max      30.2310
_cell_measurement_theta_min      3.4360
_cell_volume                     5207.49(10)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2017)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2017)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2017)
;
_computing_molecular_graphics
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
SHELXL2016 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2014 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      122.99(10)
_diffrn_detector_area_resol_mean 15.9702
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type
'Rigaku Oxford DiffractionSuperNova Single source at offset/far, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0320
_diffrn_reflns_av_unetI/netI     0.0354
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            33230
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.103
_diffrn_reflns_theta_min         3.330
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.698
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.798
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2017)
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.600
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2536
_exptl_crystal_size_max          0.157
_exptl_crystal_size_mid          0.124
_exptl_crystal_size_min          0.121
_refine_diff_density_max         0.938
_refine_diff_density_min         -0.539
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     586
_refine_ls_number_reflns         11436
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0390
_refine_ls_R_factor_gt           0.0297
_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/[\s^2^(Fo^2^)+(0.0225P)^2^+4.0699P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0617
_refine_ls_wR_factor_ref         0.0654
_reflns_number_gt                9742
_reflns_number_total             11436
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm4112sup1.cif
_cod_data_source_block           I
_cod_database_code               1552332
_shelx_hkl_checksum              64150
_shelx_res_checksum              16575
_cod_database_fobs_code 1552332