A Heteroaromatically Functionalized Hexamolybdate
Healey, Merinda; Best, Stephen; Goerigk, Lars; Ritchie, Chris; Inorganics 3 (2015) 82–; doi:10.3390/inorganics3020082

data_1520328
_publ_section_title
;
 A Heteroaromatically Functionalized Hexamolybdate
;
_journal_issue                   2
_journal_name_full               Inorganics
_journal_page_first              82
_journal_paper_doi               10.3390/inorganics3020082
_journal_volume                  3
_journal_year                    2015
_chemical_formula_moiety         'C26 H22 Br N S'
_chemical_formula_sum            'C26 H22 Br N S'
_chemical_formula_weight         460.41
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2015-03-19
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 101.954(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.5989(5)
_cell_length_b                   11.5694(5)
_cell_length_c                   15.2670(6)
_cell_measurement_reflns_used    3914
_cell_measurement_temperature    130.10(10)
_cell_measurement_theta_max      29.0390
_cell_measurement_theta_min      3.7800
_cell_volume                     2177.09(16)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      293.18(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2273
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.877
_diffrn_measurement_details
;
  1 omega  -27.00   92.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       13.0310   19.0000 -120.0000 119

  2 omega  -22.00    4.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       13.0310  -38.0000  -90.0000 26

  3 omega  -20.00   22.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.2653  -99.0000   60.0000 42

  4 omega  -97.00  -55.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.2653  178.0000 -180.0000 42
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0390004000
_diffrn_orient_matrix_UB_12      0.0447969000
_diffrn_orient_matrix_UB_13      0.0032805000
_diffrn_orient_matrix_UB_21      -0.0418417000
_diffrn_orient_matrix_UB_22      0.0419187000
_diffrn_orient_matrix_UB_23      -0.0032345000
_diffrn_orient_matrix_UB_31      0.0063525000
_diffrn_orient_matrix_UB_32      -0.0002718000
_diffrn_orient_matrix_UB_33      0.0472200000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0434
_diffrn_reflns_av_unetI/netI     0.0664
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.877
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            13627
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.877
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.228
_diffrn_reflns_theta_min         2.937
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.996
_exptl_absorpt_correction_T_max  0.845
_exptl_absorpt_correction_T_min  0.620
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.405
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.411
_exptl_crystal_size_mid          0.2013
_exptl_crystal_size_min          0.0893
_refine_diff_density_max         0.770
_refine_diff_density_min         -0.862
_refine_diff_density_rms         0.268
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.151
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     265
_refine_ls_number_reflns         5687
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.151
_refine_ls_R_factor_all          0.0769
_refine_ls_R_factor_gt           0.0497
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0882P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1394
_refine_ls_wR_factor_ref         0.1727
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4272
_reflns_number_total             5687
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            s2.cif
_cod_data_source_block           mh1-139-2
_cod_original_cell_volume        2177.07(16)
_cod_database_code               1520328
_chemical_oxdiff_formula         'C26 H22 N S Br'
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C16(H16), C18(H18), C23(H23)
2.b Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C26(H26A,H26B,H26C)
;
_shelx_res_checksum              64472
_shelx_hkl_checksum              46781
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2015-03-16
_olex2_submission_special_instructions 'No special instructions were received'