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_4329319
_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            'C20 H16 Br Mn2 N11 O6'
_chemical_formula_weight         696.23
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.354(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            6
_cell_length_a                   16.232(7)
_cell_length_b                   9.622(4)
_cell_length_c                   27.200(9)
_cell_measurement_reflns_used    959
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.475
_cell_measurement_theta_min      2.765
_cell_volume                     4213(3)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_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      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w 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  0.0735
_diffrn_reflns_av_sigmaI/netI    0.0638
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            26351
_diffrn_reflns_theta_full        23.29
_diffrn_reflns_theta_max         23.29
_diffrn_reflns_theta_min         1.26
_exptl_absorpt_coefficient_mu    2.377
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.748043
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            YELLOW
_exptl_crystal_density_diffrn    1.646
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             2076
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.696
_refine_diff_density_min         -0.826
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     542
_refine_ls_number_reflns         6052
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.1024
_refine_ls_R_factor_gt           0.0760
_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^)+(0.0607P)^2^+23.1651P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1656
_refine_ls_wR_factor_ref         0.1763
_reflns_number_gt                4546
_reflns_number_total             6052
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic202631c_si_002_4.cif
_cod_data_source_block           Compound_3_ma369bm
_cod_database_code               4329319