Metallathiacrown Ethers: Synthesis and Characterization of Transition-Metal Complexes Containing α,ω-Bis(phosphite)-Polythioether Ligands and an Evaluation of Their Soft Metal Binding Capabilities
Martin, Justin R.; Lucius, Aaron L.; Gray, Gary M.; Organometallics 34 (2015) 4605–; doi:10.1021/acs.organomet.5b00693

data_4086273
_publ_section_title
;
 Metallathiacrown Ethers: Synthesis and Characterization of
 Transition-Metal Complexes Containing \a,\w-Bis(phosphite)-Polythioether
 Ligands and an Evaluation of Their Soft Metal Binding Capabilities
;
_journal_issue                   18
_journal_name_full               Organometallics
_journal_page_first              4605
_journal_paper_doi               10.1021/acs.organomet.5b00693
_journal_volume                  34
_journal_year                    2015
_chemical_formula_sum            'C38 H28 Mo O10 P2 S2'
_chemical_formula_weight         866.60
_chemical_name_systematic
;
 ?
;
_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
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 94.8640(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.9707(3)
_cell_length_b                   20.5722(4)
_cell_length_c                   13.4438(3)
_cell_measurement_reflns_used    6479
_cell_measurement_temperature    102(2)
_cell_measurement_theta_max      68.36
_cell_measurement_theta_min      3.94
_cell_volume                     3574.37(13)
_computing_cell_refinement       'SAINT (Bruker AXS, 2012)'
_computing_data_collection       'APEX2 (Version 2012.10-0)'
_computing_data_reduction        'SADABS V2012/1 (Bruker AXS)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXTL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      102(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker SMART BREEZE CCD'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0368
_diffrn_reflns_av_unetI/netI     0.0285
_diffrn_reflns_laue_measured_fraction_full 0.989
_diffrn_reflns_laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            31466
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.363
_diffrn_reflns_theta_min         3.938
_diffrn_source                   'fine-focused sealed tube'
_exptl_absorpt_coefficient_mu    5.458
_exptl_absorpt_correction_T_max  0.72280
_exptl_absorpt_correction_T_min  0.47311
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS 2013'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.610
_exptl_crystal_density_meas      ?
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             1760
_exptl_crystal_size_max          0.262
_exptl_crystal_size_mid          0.164
_exptl_crystal_size_min          0.085
_refine_diff_density_max         0.499
_refine_diff_density_min         -0.450
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     478
_refine_ls_number_reflns         6479
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0292
_refine_ls_R_factor_gt           0.0281
_refine_ls_shift/su_max          0.043
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0357P)^2^+3.6510P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0728
_refine_ls_wR_factor_ref         0.0736
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6220
_reflns_number_total             6479
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00693_si_002.cif
_cod_data_source_block           jrmii1112a_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 
;
_cod_database_code               4086273
_shelx_estimated_absorpt_t_min   0.329
_shelx_estimated_absorpt_t_max   0.654
_shelxl_version_number           2013-4
_shelx_res_checksum              21736
_shelx_hkl_checksum              52816