Comparison of molybdenum and rhenium oxo bis-pyrazine-dithiolene complexes - in search of an alternative metal centre for molybdenum cofactor models.
Chrysochos, Nicolas; Ahmadi, Mohsen; Wahlefeld, Stefan; Rippers, Yvonne; Zebger, Ingo; Mroginski, Maria Andrea; Schulzke, Carola; Dalton transactions (Cambridge, England : 2003) 48 (2019) 2701–2714; doi:10.1039/c8dt04237c

data_7048749
_publ_section_title
;
 Comparison of molybdenum and rhenium oxo bis-pyrazine-dithiolene
 complexes - in search of an alternative metal centre for molybdenum
 cofactor models.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2701
_journal_page_last               2714
_journal_paper_doi               10.1039/c8dt04237c
_journal_volume                  48
_journal_year                    2019
_chemical_formula_sum            'C24 H46 Mo N6 O2 S4'
_chemical_formula_weight         674.85
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2018-10-15 deposited with the CCDC.
2019-01-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.25(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.5168(19)
_cell_length_b                   13.590(3)
_cell_length_c                   12.011(2)
_cell_measurement_reflns_used    17863
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      58.9
_cell_measurement_theta_min      3.0
_cell_volume                     1549.2(5)
_computing_cell_refinement       'X-Area by STOE & Cie GmbH 2010'
_computing_data_reduction        'X-Area by STOE & Cie GmbH 2010'
_computing_molecular_graphics    'XP Version 5.1 by Bruker AXS 1998'
_computing_publication_material  'CIFTAB (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2016 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT-2016 (Sheldrick, 2016)'
_diffrn_ambient_temperature      170(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'STOE IPDS2T'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0714
_diffrn_reflns_av_unetI/netI     0.0500
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            17816
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.457
_diffrn_reflns_theta_min         1.700
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.725
_exptl_absorpt_correction_T_max  0.9879
_exptl_absorpt_correction_T_min  0.9086
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'face indexed'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.447
_exptl_crystal_description       block
_exptl_crystal_F_000             708
_exptl_crystal_size_max          0.448
_exptl_crystal_size_mid          0.432
_exptl_crystal_size_min          0.337
_refine_diff_density_max         0.930
_refine_diff_density_min         -1.419
_refine_diff_density_rms         0.100
_refine_ls_abs_structure_details
;
 Flack x determined using 3565 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.02(3)
_refine_ls_extinction_coef       0.0140(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   0.913
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     351
_refine_ls_number_reflns         8328
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.913
_refine_ls_R_factor_all          0.0345
_refine_ls_R_factor_gt           0.0319
_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^)+(0.0699P)^2^+1.2556P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0863
_refine_ls_wR_factor_ref         0.0949
_reflns_Friedel_coverage         0.880
_reflns_Friedel_fraction_full    0.982
_reflns_Friedel_fraction_max     0.946
_reflns_number_gt                8014
_reflns_number_total             8328
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04237c2.cif
_cod_data_source_block           NCS200C
_cod_depositor_comments
'Adding full bibliography for 7048748--7048749.cif.'
_cod_database_code               7048749
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.737
_shelx_estimated_absorpt_t_max   0.792
_exptl_absorpt_special_details
; 
programs X-Red32 and X-Shape by STOE & Cie GmbH 2010
;
_shelx_res_checksum              24696