Syntheses and properties of hydride‒cyanamide and derived hydrogen-cyanamide complexes of molybdenum(IV). Crystal structure of [MoH2(NCNH2)2(Ph2PCH2CH2PPh2)2][BF4]2
Luísa M. D. R. S. Martins; Elisabete C. B. A. Alegria; David L. Hughes; João J. R. Fraústo da Silva; Armando J. L. Pombeiro; Dalton Trans.  (2003) 3743–3750; doi:10.1039/b306368b

data_7013310
_publ_section_title
;
 Syntheses and properties of hydride--cyanamide and derived
 hydrogen-cyanamide complexes of molybdenum(IV). Crystal structure of
 [MoH2(NCNH2)2(Ph2PCH2CH2PPh2)2][BF4]2
;
_journal_issue                   19
_journal_name_full               'Dalton Trans.'
_journal_page_first              3743
_journal_page_last               3750
_journal_paper_doi               10.1039/b306368b
_journal_year                    2003
_chemical_formula_moiety         'C54 H54 Mo N4 P4, 2(B F4), C4 H8 O, (?)'
_chemical_formula_structural     '[Mo(H)2(NCNH2)2(dppe)2](BF4)2.thf.(solvent?)'
_chemical_formula_sum            'C58 H62 B2 F8 Mo N4 O P4'
_chemical_formula_weight         1224.56
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.06(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   32.620(5)
_cell_length_b                   14.848(2)
_cell_length_c                   12.440(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      9
_cell_measurement_theta_min      7
_cell_volume                     5991.5(19)
_computing_cell_refinement       'CAD4/EXPRESS (Enraf-Nonius, 1992)'
_computing_data_collection       'CAD4/EXPRESS (Enraf-Nonius, 1992)'
_computing_data_reduction        'CAD4 (Hursthouse, 1976)'
_computing_molecular_graphics    'ORTEP (Johnson, 1971)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       'Enraf-Nonius CAD4 diffractometer'
_diffrn_measurement_method       'scintillation counter; \w/\q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.073
_diffrn_reflns_av_sigmaI/netI    0.1256
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4416
_diffrn_reflns_theta_full        17.98
_diffrn_reflns_theta_max         17.98
_diffrn_reflns_theta_min         1.51
_diffrn_standards_decay_%        21.9
_diffrn_standards_interval_time  '10000 s'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.393
_exptl_absorpt_correction_T_max  0.015
_exptl_absorpt_correction_T_min  0.006
_exptl_absorpt_correction_type   'semi-empirical psi-scans'
_exptl_absorpt_process_details
;
EMPABS, (Sheldrick et al,' 1977)
;
_exptl_crystal_colour            'dull yellow'
_exptl_crystal_density_diffrn    1.358
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelipipeds
_exptl_crystal_F_000             2520
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.444
_refine_diff_density_min         -0.371
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     692
_refine_ls_number_reflns         4060
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.1559
_refine_ls_R_factor_gt           0.0940
_refine_ls_shift/su_max          0.095
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1529P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2333
_refine_ls_wR_factor_ref         0.2903
_reflns_number_gt                1942
_reflns_number_total             4060
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            b306368b.txt
_cod_data_source_block           luisa1
_cod_original_sg_symbol_H-M      'P 21/a'
_cod_database_code               7013310