Large Ligand Folding Distortion in an Oxomolybdenum Donor-Acceptor Complex.
Yang, Jing; Mogesa, Benjamin; Basu, Partha; Kirk, Martin L.; Inorganic chemistry 55 (2016) 785–793; doi:10.1021/acs.inorgchem.5b02252

data_4344603
_publ_section_title
;
 Large Ligand Folding Distortion in an Oxomolybdenum Donor-Acceptor
 Complex.
;
_journal_issue                   2
_journal_name_full               'Inorganic chemistry'
_journal_page_first              785
_journal_page_last               793
_journal_paper_doi               10.1021/acs.inorgchem.5b02252
_journal_volume                  55
_journal_year                    2016
_chemical_formula_sum            'C22 H28 Mo N2 O S4'
_chemical_formula_weight         560.64
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-11-06 # Formatted by publCIF

;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   36.3946(5)
_cell_length_b                   36.3946(5)
_cell_length_c                   10.0644(2)
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      29.689
_cell_measurement_theta_min      2.240
_cell_volume                     11545.0(3)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.833
_diffrn_measured_fraction_theta_max 0.888
_diffrn_measurement_device_type  'Bruker Smart ApexII'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_unetI/netI     0.0696
_diffrn_reflns_laue_measured_fraction_full 0.833
_diffrn_reflns_laue_measured_fraction_max 0.888
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -50
_diffrn_reflns_limit_k_max       50
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11144
_diffrn_reflns_point_group_measured_fraction_full 0.833
_diffrn_reflns_point_group_measured_fraction_max 0.888
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.703
_diffrn_reflns_theta_min         1.119
_exptl_absorpt_coefficient_mu    0.853
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2002)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.451
_exptl_crystal_description       rhomboid
_exptl_crystal_F_000             5184
_exptl_crystal_size_max          0.640
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.120
_exptl_transmission_factor_max   0.9045
_exptl_transmission_factor_min   0.832
_refine_diff_density_max         1.215
_refine_diff_density_min         -1.108
_refine_diff_density_rms         0.248
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.425
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     276
_refine_ls_number_reflns         5657
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.425
_refine_ls_R_factor_all          0.1200
_refine_ls_R_factor_gt           0.0824
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1919
_refine_ls_wR_factor_ref         0.2332
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3936
_reflns_number_total             5657
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02252_si_001.cif
_cod_data_source_block           detwinned
_cod_depositor_comments
;

2020-09-02
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_weight         420.48
_cod_original_formula_units_Z            24
_cod_original_cell_volume        11545.0(4)
_cod_original_formula_sum        'C16.50 H21 Mo0.75 N1.50 O0.75 S3'
_cod_database_code               4344603
_publcif_datablock.id            {96c25149-c023-497b-991a-614f25da0810}
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.611
_shelx_estimated_absorpt_t_max   0.905
_plat019_alert_1_b
;
PROBLEM: diffrn_measured_fraction_theta_full/_max < 1.0
RESPONSE:  This error is the result the crystal weakly 
diffracting.
;
_plat028_alert_3_b
;
PROBLEM: diffrn_measured_fraction_theta_max 0.888
RESPONSE:  This error is the result the crystal weakly 
diffracting.
;
_shelx_res_checksum              45649
_shelx_hkl_checksum              47079
_publcif_info_exptl_table_max_cols 4
_publcif_info_exptl_table_use_headnotes n