Synthesis and Molecular and Electronic Structure of an Unusual Paramagnetic Borohydride Complex Mo(NAr)2(PMe3)2(η2-BH4)
Andrey Y. Khalimon; Jason P. Holland; Radoslaw M. Kowalczyk; Eric J. L. McInnes; Jennifer C. Green; Philip Mountford; Georgii I. Nikonov; Inorganic Chemistry 47 (2008) 999–1006; doi:10.1021/ic701826v

data_4304342
_publ_section_title
;
Synthesis and Molecular and Electronic Structure of an Unusual Paramagnetic
Borohydride Complex Mo(NAr)2(PMe3)2(\h2-BH4)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              999
_journal_page_last               1006
_journal_paper_doi               10.1021/ic701826v
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C30 H56 B1 Mo1 N2 P2'
_chemical_formula_sum            'C30 H56 B Mo N2 P2'
_chemical_formula_weight         613.49
_chemical_name_systematic
;
Mo(NAr)2(PMe3)2BH4
;
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             06-10-17
_audit_creation_method           CRYSTALS_ver_12.80
_cell_angle_alpha                102.8021(14)
_cell_angle_beta                 93.3190(14)
_cell_angle_gamma                107.7986(11)
_cell_formula_units_Z            2
_cell_length_a                   11.2581(3)
_cell_length_b                   12.8096(4)
_cell_length_c                   13.0998(4)
_cell_measurement_reflns_used    7023
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     1737.88(9)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'Nonius (1997-2001). COLLECT.'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.019
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13397
_diffrn_reflns_theta_full        26.417
_diffrn_reflns_theta_max         27.518
_diffrn_reflns_theta_min         5.111
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.489
_exptl_absorpt_correction_T_max  0.91
_exptl_absorpt_correction_T_min  0.89
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.172
_exptl_crystal_description       block
_exptl_crystal_F_000             654
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.01
_refine_diff_density_min         -0.92
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9254
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     338
_refine_ls_number_reflns         7894
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.0632
_refine_ls_R_factor_gt           0.0452
_refine_ls_shift/su_max          0.009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(F^2^) + 0.04 + 2.61P] 
where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1077
_refine_ls_wR_factor_gt          0.1011
_refine_ls_wR_factor_ref         0.1077
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              16
_reflns_limit_k_min              -16
_reflns_limit_l_max              17
_reflns_limit_l_min              0
_reflns_number_gt                6221
_reflns_number_total             7894
_reflns_threshold_expression     I>2.00u(I)
_oxford_refine_ls_scale          0.3545(3)
_oxford_structure_analysis_title GIN16
_cod_data_source_file            ic701826v-file003.cif
_cod_data_source_block           compound1
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C30 H56 B1 Mo1 N2 P2'
_cod_database_code               4304342