The first ReI organometallic complex with an organoimido-polyoxometalate ligand
Hermosilla-Ibáñez, Patricio; Wrighton-Araneda, Kerry; Prado, Gaspar; Paredes-Garcia, Veronica; Pizarro, Nancy Alejandra; Vega, Andres; Venegas-Yazigi, Diego; Dalton Trans.  (2017) –; doi:10.1039/C7DT01633F

data_7043281
_publ_section_title
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 The first ReI organometallic complex with an organoimido-polyoxometalate
 ligand
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_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01633F
_journal_year                    2017
_chemical_formula_moiety         'C9 H8 Mo6 N4 O18, 2(C16 H36 N)'
_chemical_formula_sum            'C41 H80 Mo6 N6 O18'
_chemical_formula_weight         1520.75
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
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2017-05-31 deposited with the CCDC.
2017-06-08 downloaded from the CCDC.
;
_cell_angle_alpha                85.180(3)
_cell_angle_beta                 84.602(3)
_cell_angle_gamma                82.019(3)
_cell_formula_units_Z            2
_cell_length_a                   11.835(3)
_cell_length_b                   14.997(4)
_cell_length_c                   16.445(4)
_cell_measurement_reflns_used    5737
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.330
_cell_measurement_theta_min      2.227
_cell_volume                     2870.3(13)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Smart Apex II'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1095
_diffrn_reflns_av_unetI/netI     0.1181
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            92492
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.000
_diffrn_reflns_theta_min         2.227
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.340
_exptl_absorpt_correction_T_max  0.459
_exptl_absorpt_correction_T_min  0.378
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            ORANGE
_exptl_crystal_density_diffrn    1.760
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1528
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.574
_refine_diff_density_min         -0.561
_refine_diff_density_rms         0.097
_refine_ls_abs_structure_details
;
 Flack x determined using 4234 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.02(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1367
_refine_ls_number_reflns         24951
_refine_ls_number_restraints     263
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.1506
_refine_ls_R_factor_gt           0.0604
_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^)+(0.0423P)^2^+2.9793P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1093
_refine_ls_wR_factor_ref         0.1445
_reflns_Friedel_coverage         0.999
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                12294
_reflns_number_total             24951
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01633f2.cif
_cod_data_source_block           POM-METRIAZOL-P1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'EMPIRICAL' changed to
'empirical' 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 
;
_cod_original_cell_volume        2870.4(12)
_cod_database_code               7043281
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              63834