Metathetical Exchange between Metal-Metal Triple Bonds.
Queen, Joshua D.; Phung, Alice C.; Caputo, Christine A.; Fettinger, James C.; Power, Philip P.; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.9b13604

data_4134042
_publ_section_title
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 Metathetical Exchange between Metal-Metal Triple Bonds.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.9b13604
_journal_year                    2020
_chemical_formula_moiety         'C37 H42 Ge Mo O2'
_chemical_formula_sum            'C37 H42 Ge Mo O2'
_chemical_formula_weight         687.23
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-09-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-11-04 deposited with the CCDC.	2019-12-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.4620(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.3692(9)
_cell_length_b                   16.3298(12)
_cell_length_c                   18.4110(14)
_cell_measurement_reflns_used    9981
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      30.51
_cell_measurement_theta_min      2.30
_cell_volume                     3337.6(4)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      90.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0303
_diffrn_reflns_av_unetI/netI     0.0242
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            38995
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.558
_diffrn_reflns_theta_min         2.218
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.306
_exptl_absorpt_correction_T_max  0.6881
_exptl_absorpt_correction_T_min  0.6307
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0615 before and 0.0322 after correction. The Ratio of minimum to maximum transmission is 0.9166. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_description       Block
_exptl_crystal_F_000             1416
_exptl_crystal_size_max          0.239
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.539
_refine_diff_density_min         -0.413
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     378
_refine_ls_number_reflns         10223
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0314
_refine_ls_R_factor_gt           0.0243
_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^)+(0.0278P)^2^+1.5022P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0576
_refine_ls_wR_factor_ref         0.0604
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8829
_reflns_number_total             10223
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b13604_si_003.cif
_cod_data_source_block           jq105fmi
_cod_database_code               4134042
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.818
_shelx_estimated_absorpt_t_min   0.745
_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 Ternary CH refined with riding coordinates:
 C16(H16), C13(H13), C28(H28), C25(H25), C31(H31), C32(H32), C33(H33),
 C34(H34), C35(H35)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C11(H11), C10(H10), C9(H9), C23(H23), C22(H22),
 C21(H21)
2.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C17(H17A,H17B,H17C), C15(H15A,H15B,H15C), C14(H14A,H14B,
 H14C), C30(H30A,H30B,H30C), C29(H29A,H29B,H29C), C27(H27A,H27B,H27C), C26(H26A,
 H26B,H26C)
;
_shelx_res_checksum              16202
_shelx_hkl_checksum              69012
_olex2_submission_special_instructions 'No special instructions were received'