Unusual coordination of tetrylenes to molybdenum carbonyl fragments
Felicitas Lips; Joshua D. Queen; James C. Fettinger; Philip P. Power; Chem.Commun. 50 (2014) 5561–; doi:10.1039/C4CC00999A

data_7113316
_publ_section_title
;
 Unusual coordination of tetrylenes to molybdenum carbonyl fragments
;
_journal_name_full               Chem.Commun.
_journal_page_first              5561
_journal_paper_doi               10.1039/C4CC00999A
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         'C55 H58 Ge Mo O4 S2'
_chemical_formula_sum            'C55 H58 Ge Mo O4 S2'
_chemical_formula_weight         1015.66
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2012
_cell_angle_alpha                90
_cell_angle_beta                 109.3022(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.8239(2)
_cell_length_b                   13.6512(2)
_cell_length_c                   23.5101(4)
_cell_measurement_reflns_used    3852
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      71.42
_cell_measurement_theta_min      21.35
_cell_volume                     4793.07(12)
_computing_cell_refinement       'SAINT (8.27b) (Bruker, 2012)'
_computing_data_collection       'Apex2 (2013.6-2) (Bruker, 2013)'
_computing_data_reduction        'SAINT (8.27b) (Bruker, 2012)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_computing_structure_solution    'SHELXT (Sheldrick, 2013)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_unetI/netI     0.0480
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9147
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         71.477
_diffrn_reflns_theta_min         2.959
_exptl_absorpt_coefficient_mu    4.083
_exptl_absorpt_correction_T_max  0.6897
_exptl_absorpt_correction_T_min  0.4974
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS V2012/1 (Sheldrick, 2012)'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_description       Block
_exptl_crystal_F_000             2104
_exptl_crystal_size_max          0.181
_exptl_crystal_size_mid          0.109
_exptl_crystal_size_min          0.102
_refine_diff_density_max         1.677
_refine_diff_density_min         -1.147
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     581
_refine_ls_number_reflns         9147
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0605
_refine_ls_R_factor_gt           0.0519
_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^)+(0.1071P)^2^+3.1223P] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1491
_refine_ls_wR_factor_ref         0.1579
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7795
_reflns_number_total             9147
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cc00999a2.cif
_cod_data_source_block           fl134tw351_compound3
_cod_original_cell_volume        4793.06(12)
_cod_database_code               7113316
_shelx_estimated_absorpt_t_min   0.525
_shelx_estimated_absorpt_t_max   0.681
_shelxl_version_number           2012-9
_shelx_res_checksum              20759