Crystal structures and hydrogen-bonding analysis of a series of solvated ammonium salts of molybdenum(II) chloride clusters
Johnston, Dean H.; Agho, Ikponmwosa; Acta Crystallographica Section E 75 (2019) 1705–1711; doi:10.1107/S205698901901380X

data_2243142
_publ_section_title
;
 Crystal structures and hydrogen-bonding analysis of a series of solvated
 ammonium salts of molybdenum(II) chloride clusters
;
_journal_coeditor_code           EB2023
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1705
_journal_page_last               1711
_journal_paper_doi               10.1107/S205698901901380X
_journal_volume                  75
_journal_year                    2019
_chemical_formula_iupac          '(C12 H18 N2) [Mo6 Cl8 Cl6], 3C3 H6 O'
_chemical_formula_moiety         'C12 H18 N2 2+, Cl14 Mo6 2-, 3(C3 H6 O)'
_chemical_formula_sum            'C21 H36 Cl14 Mo6 N2 O3'
_chemical_formula_weight         1436.46
_chemical_name_systematic
;
<i>N</i>,<i>N</i>'-(1,4-Phenylene)bis(propan-2-iminium)
octa-\m~3~-chlorido-hexachlorido-<i>octahedro</i>-hexamolybdate acetone
trisolvate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     heavy
_cell_angle_alpha                64.933(6)
_cell_angle_beta                 71.174(6)
_cell_angle_gamma                75.440(6)
_cell_formula_units_Z            1
_cell_length_a                   9.451(2)
_cell_length_b                   11.236(3)
_cell_length_c                   11.712(3)
_cell_measurement_reflns_used    5309
_cell_measurement_temperature    200.0
_cell_measurement_theta_max      25.09
_cell_measurement_theta_min      2.24
_cell_volume                     1056.7(5)
_computing_cell_refinement
;
SAINT (Bruker, 2012)
;
_computing_data_collection
;
APEX2 (Bruker, 2012)
;
_computing_data_reduction
;
SAINT (Bruker, 2012)
;
_computing_molecular_graphics
;
<i>CrystalMaker</i> (Palmer, 2019) and <i>CrystalExplorer</i>
(Spackman & Jayatilaka, 2009)
;
_computing_publication_material
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009) and
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS (Sheldrick, 2008)
;
_diffrn_ambient_temperature      200.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.3330
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART X2S benchtop'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_av_unetI/netI     0.0320
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            10036
_diffrn_reflns_theta_full        25.147
_diffrn_reflns_theta_max         25.147
_diffrn_reflns_theta_min         2.638
_diffrn_source                   'sealed microfocus source'
_diffrn_source_current           1.0
_diffrn_source_power             0.04991
_diffrn_source_voltage           49.91
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.640
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.4904
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2012)
;
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_density_diffrn    2.257
_exptl_crystal_description       block
_exptl_crystal_F_000             690
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.963
_refine_diff_density_min         -0.820
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         3692
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0303
_refine_ls_R_factor_gt           0.0252
_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^)+(0.0347P)^2^+0.3989P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0649
_refine_ls_wR_factor_ref         0.0681
_reflns_number_gt                3220
_reflns_number_total             3692
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            eb2023sup1.cif
_cod_data_source_block           3
_cod_database_code               2243142
_shelx_estimated_absorpt_t_min   0.325
_shelx_estimated_absorpt_t_max   0.620
_shelx_res_checksum              49310
_cod_database_fobs_code 2243142