[Ge9{M(CO)5}3]4-: Electrophilic Addition of M(CO)5 and [E9]4- Zintl anions (M = Cr, Mo, W) †
Wang, LuLu; Wang, Yi; li, zhenyu; Ruan, Huapeng; Xu, Li; Dalton Trans.  (2017) –; doi:10.1039/C7DT01123G

data_7042751
_publ_section_title
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 [Ge9{M(CO)5}3]4-: Electrophilic Addition of M(CO)5 and [E9]4- Zintl
 anions (M = Cr, Mo, W) &#x2020;
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_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01123G
_journal_year                    2017
_chemical_formula_sum            'C69 H96 Ge9 K4 N6 O39 W3'
_chemical_formula_weight         2994.78
_chemical_name_systematic
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 ? 
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_chemical_properties_physical
', Air-sensitive,Moisture-sensitive,Oxygen-sensitive'
_space_group_IT_number           176
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-P 6c'
_symmetry_space_group_name_H-M   'P 63/m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2017-04-10 deposited with the CCDC.
2017-04-21 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   19.7716(9)
_cell_length_b                   19.7716(9)
_cell_length_c                   16.5975(15)
_cell_measurement_reflns_used    15710
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.5593
_cell_measurement_theta_min      2.0477
_cell_volume                     5619.0(6)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  Mercury70
_diffrn_measurement_method       CCD_Profile_fitting
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0434
_diffrn_reflns_av_sigmaI/netI    0.0188
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            44487
_diffrn_reflns_theta_full        27.70
_diffrn_reflns_theta_max         27.70
_diffrn_reflns_theta_min         2.38
_exptl_absorpt_coefficient_mu    5.647
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7129
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    1.770
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             2900
_exptl_crystal_size_max          0.3000
_exptl_crystal_size_mid          0.1000
_exptl_crystal_size_min          0.1000
_refine_diff_density_max         1.209
_refine_diff_density_min         -0.806
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.184
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         4403
_refine_ls_number_restraints     74
_refine_ls_restrained_S_all      1.200
_refine_ls_R_factor_all          0.0681
_refine_ls_R_factor_gt           0.0646
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+24.2442P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1277
_refine_ls_wR_factor_ref         0.1296
_reflns_number_gt                4169
_reflns_number_total             4403
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7dt01123g2.cif
_cod_data_source_block           a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Hexagonal' changed to 'hexagonal'
according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
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_cod_original_sg_symbol_H-M      P6(3)/m
_cod_database_code               7042751