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_2243140
_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          '(C6 H8 N)2 [Mo6 Cl8 Cl6], 4C3 H7 N O'
_chemical_formula_moiety         '2(C6 H8 N +), Cl14 Mo6 2-, 4(C3 H7 N O)'
_chemical_formula_sum            'C24 H44 Cl14 Mo6 N6 O4'
_chemical_formula_weight         1552.59
_chemical_name_systematic
;
Bis(anilinium)
octa-\m~3~-chlorido-hexachlorido-<i>octahedro</i>-hexamolybdate
<i>N</i>,<i>N</i>-dimethylformamide tetrasolvate
;
_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     direct
_cell_angle_alpha                104.606(3)
_cell_angle_beta                 90.709(3)
_cell_angle_gamma                103.146(3)
_cell_formula_units_Z            1
_cell_length_a                   9.9813(11)
_cell_length_b                   10.6074(13)
_cell_length_c                   12.1686(15)
_cell_measurement_reflns_used    7006
_cell_measurement_temperature    200
_cell_measurement_theta_max      25.049
_cell_measurement_theta_min      2.308
_cell_volume                     1210.7(3)
_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 0.982
_diffrn_measured_fraction_theta_max 0.982
_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  0.0256
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11709
_diffrn_reflns_theta_full        25.102
_diffrn_reflns_theta_max         25.102
_diffrn_reflns_theta_min         2.308
_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    2.316
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.4984
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2012)
;
_exptl_crystal_colour            'clear orangish yellow'
_exptl_crystal_density_diffrn    2.129
_exptl_crystal_description       plate
_exptl_crystal_F_000             752
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.46
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.360
_refine_diff_density_min         -0.540
_refine_ls_extinction_coef       0.0096(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2018 (Sheldrick, 2015)
;
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     258
_refine_ls_number_reflns         4245
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0219
_refine_ls_R_factor_gt           0.0186
_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^)+(0.0123P)^2^+0.5808P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0440
_refine_ls_wR_factor_ref         0.0457
_reflns_number_gt                3834
_reflns_number_total             4245
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            eb2023sup1.cif
_cod_data_source_block           1
_cod_database_code               2243140
_shelx_estimated_absorpt_t_min   0.403
_shelx_estimated_absorpt_t_max   0.769
_shelx_res_checksum              24947
_cod_database_fobs_code 2243140