Synthesis and structure of mixed carboxylate-aminopyridinate and -amidinate complexes of dimolybdenum and ditungsten
Irene Mendoza; Natalia Curado; Mario Carrasco; Eleuterio Alvarez; Riccardo Peloso; Amor Rodriguez; Ernesto Carmona; Inorganica Chimica Acta 424 (2015) 120–128; doi:

data_1518802
_publ_section_title
;
 Synthesis and structure of mixed carboxylate-aminopyridinate and
 -amidinate complexes of dimolybdenum and ditungsten
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              120
_journal_page_last               128
_journal_volume                  424
_journal_year                    2015
_chemical_formula_moiety         'C62 H74 F6 Mo2 N4 O4, C6 H14'
_chemical_formula_sum            'C68 H88 F6 Mo2 N4 O4'
_chemical_formula_weight         1331.30
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 107.660(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.0604(11)
_cell_length_b                   13.6420(6)
_cell_length_c                   23.0026(10)
_cell_measurement_reflns_used    9883
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.39
_cell_measurement_theta_min      2.35
_cell_volume                     6596.3(5)
_computing_cell_refinement       'APEX2 Software Suite (Bruker, 2007)'
_computing_data_collection       'APEX2 Software Suite (Bruker, 2007)'
_computing_data_reduction        'APEX2 Software Suite (Bruker, 2007)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL and publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2002 (Burla et al., 2003)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
;
 Bruker-Nonius X8kappa APEX II CCD area detector
;
_diffrn_measurement_method       'phi and omega scans with narrow frames'
_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  0.0361
_diffrn_reflns_av_sigmaI/netI    0.0153
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            77746
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         1.78
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.446
_exptl_absorpt_correction_T_max  0.8333
_exptl_absorpt_correction_T_min  0.8041
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
program SADABS, Bruker (2001).
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.341
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2776
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.41
_exptl_crystal_size_min          0.41
_refine_diff_density_max         0.727
_refine_diff_density_min         -0.570
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     389
_refine_ls_number_reflns         5969
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0384
_refine_ls_R_factor_gt           0.0309
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0392P)^2^+13.3306P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0781
_refine_ls_wR_factor_ref         0.0824
_reflns_number_gt                5273
_reflns_number_total             5969
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2015-424-120-128-4.cif
_cod_data_source_block           2c
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 2827 2014-09-09 07:05:25Z andrius 
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               1518802