Coordination versus Coupling of Dicyanamide in Molybdenum and Manganese Pyrazole Complexes
Marta Arroyo; Patricia Gómez-Iglesias; Jose Miguel Martín-Alvarez; Celedonio M. Alvarez; Daniel Miguel; Fernando Villafañe; Inorganic Chemistry 51 (2012) 6070–6080; doi:10.1021/ic202631c

data_4329318
_publ_contact_author
;
     FERNANDO VILLAFA\~NE
     IU CINQUIMA/Qu\'imica Inorg\'anica
     Facultad de Ciencias
     Universidad de Valladolid
     C/ Prado de la Magdalena s/n
     47005 Valladolid
     SPAIN
;
_publ_contact_author_email       fervilla@qi.uva.es
_publ_contact_author_fax         +34-983-423013
_publ_contact_author_phone       +34-983-184620
_publ_section_title
;
 Coordination versus Coupling of Dicyanamide in Molybdenum and Manganese
 Pyrazole Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6070
_journal_page_last               6080
_journal_paper_doi               10.1021/ic202631c
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C19 H24 Mn N7 O4'
_chemical_formula_weight         469.39
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                98.909(13)
_cell_angle_beta                 96.890(13)
_cell_angle_gamma                107.068(13)
_cell_formula_units_Z            2
_cell_length_a                   8.733(7)
_cell_length_b                   10.655(8)
_cell_length_c                   13.642(11)
_cell_measurement_reflns_used    1009
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      22.817
_cell_measurement_theta_min      2.676
_cell_volume                     1180.3(16)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.940
_diffrn_measured_fraction_theta_max 0.940
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0397
_diffrn_reflns_av_sigmaI/netI    0.0504
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11278
_diffrn_reflns_theta_full        28.59
_diffrn_reflns_theta_max         28.59
_diffrn_reflns_theta_min         1.53
_exptl_absorpt_coefficient_mu    0.597
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.368812
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            YELLOW
_exptl_crystal_density_diffrn    1.321
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             488
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.609
_refine_diff_density_min         -0.500
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.161
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         5682
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.161
_refine_ls_R_factor_all          0.0900
_refine_ls_R_factor_gt           0.0608
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0389P)^2^+1.3085P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1506
_refine_ls_wR_factor_ref         0.1609
_reflns_number_gt                3926
_reflns_number_total             5682
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic202631c_si_002_3.cif
_cod_data_source_block           Compound_2b_ma409am
_cod_database_code               4329318