#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/86/7018629.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7018629
loop_
_publ_author_name
'Weiss, Charles J.'
'Groves, Amy N.'
'Mock, Michael T.'
'Dougherty, William G.'
'Kassel, W. Scott'
'Helm, Monte L.'
'Dubois, Daniel L.'
'Bullock, R. Morris'
_publ_section_title
;
 Synthesis and reactivity of molybdenum and tungsten bis(dinitrogen)
 complexes supported by diphosphine chelates containing pendant amines.
;
_journal_issue                   15
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4517
_journal_page_last               4529
_journal_paper_doi               10.1039/c2dt12224c
_journal_volume                  41
_journal_year                    2012
_chemical_formula_sum            'C17 H31 Br Mo0.5 N P2'
_chemical_formula_weight         439.25
_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                73.2370(10)
_cell_angle_beta                 84.9840(10)
_cell_angle_gamma                85.1490(10)
_cell_formula_units_Z            2
_cell_length_a                   8.8246(4)
_cell_length_b                   10.0917(4)
_cell_length_c                   11.2789(5)
_cell_measurement_reflns_used    9902
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.17
_cell_measurement_theta_min      2.40
_cell_volume                     956.22(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω 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  0.0170
_diffrn_reflns_av_sigmaI/netI    0.0185
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            23040
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         33.19
_diffrn_reflns_theta_min         2.11
_exptl_absorpt_coefficient_mu    2.626
_exptl_absorpt_correction_T_max  0.6787
_exptl_absorpt_correction_T_min  0.5597
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.526
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             452
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.508
_refine_diff_density_min         -0.359
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     220
_refine_ls_number_reflns         7248
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0236
_refine_ls_R_factor_gt           0.0187
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0232P)²+0.2565P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0451
_refine_ls_wR_factor_ref         0.0468
_reflns_number_gt                6484
_reflns_number_total             7248
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt12224c.txt
_cod_data_source_block           trans-MoBr2(PEtNBnPEt)2_(1)
_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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C17 H31 Br Mo0.50 N P2'
_cod_database_code               7018629
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.5000 0.5000 0.5000 0.01095(3) Uani 1 2 d S . .
Br1 Br 0.692404(11) 0.661594(11) 0.534554(10) 0.01641(3) Uani 1 1 d . . .
N1 N 0.15800(10) 0.78983(9) 0.40552(8) 0.01471(15) Uani 1 1 d . . .
P1 P 0.40925(3) 0.66672(3) 0.30513(2) 0.01391(5) Uani 1 1 d . . .
P2 P 0.71740(3) 0.40047(3) 0.38886(2) 0.01196(5) Uani 1 1 d . . .
C1 C 0.4687(3) 0.8487(3) 0.2480(3) 0.0169(4) Uani 0.630(4) 1 d PU A 1
H1B H 0.4004 0.9019 0.1833 0.020 Uiso 0.630(4) 1 calc PR A 1
H1C H 0.4537 0.8908 0.3177 0.020 Uiso 0.630(4) 1 calc PR A 1
C2 C 0.6334(2) 0.86463(18) 0.19444(18) 0.0205(4) Uani 0.630(4) 1 d PU A 1
H2A H 0.6529 0.9633 0.1642 0.031 Uiso 0.630(4) 1 calc PR A 1
H2B H 0.6502 0.8230 0.1255 0.031 Uiso 0.630(4) 1 calc PR A 1
H2C H 0.7027 0.8178 0.2592 0.031 Uiso 0.630(4) 1 calc PR A 1
C1' C 0.5149(5) 0.8216(5) 0.2573(5) 0.0167(7) Uani 0.370(4) 1 d PU A 2
H1'A H 0.4862 0.8748 0.3180 0.020 Uiso 0.370(4) 1 calc PR A 2
H1'B H 0.6243 0.7919 0.2651 0.020 Uiso 0.370(4) 1 calc PR A 2
C2' C 0.4996(4) 0.9208(3) 0.1293(3) 0.0250(8) Uani 0.370(4) 1 d PU A 2
H2'A H 0.5482 1.0064 0.1237 0.038 Uiso 0.370(4) 1 calc PR A 2
H2'B H 0.3913 0.9425 0.1142 0.038 Uiso 0.370(4) 1 calc PR A 2
H2'C H 0.5491 0.8780 0.0671 0.038 Uiso 0.370(4) 1 calc PR A 2
C3 C 0.41905(13) 0.60018(13) 0.16782(11) 0.0218(2) Uani 1 1 d . A .
H3A H 0.5275 0.5747 0.1494 0.026 Uiso 1 1 calc R . .
H3B H 0.3651 0.5133 0.1923 0.026 Uiso 1 1 calc R . .
C4 C 0.35693(19) 0.6901(2) 0.04715(13) 0.0451(4) Uani 1 1 d . . .
H4A H 0.3676 0.6381 -0.0146 0.068 Uiso 1 1 calc R A .
H4B H 0.4141 0.7738 0.0163 0.068 Uiso 1 1 calc R . .
H4C H 0.2490 0.7165 0.0619 0.068 Uiso 1 1 calc R . .
C5 C 0.20426(12) 0.72019(11) 0.30977(10) 0.01716(19) Uani 1 1 d . A .
H5A H 0.1796 0.7835 0.2279 0.021 Uiso 1 1 calc R . .
H5B H 0.1449 0.6372 0.3251 0.021 Uiso 1 1 calc R . .
C6 C 0.03082(12) 0.89366(10) 0.36607(11) 0.01727(19) Uani 1 1 d . . .
H6A H -0.0143 0.9240 0.4382 0.021 Uiso 1 1 calc R . .
H6B H -0.0492 0.8509 0.3358 0.021 Uiso 1 1 calc R . .
C7 C 0.19569(13) 1.09614(11) 0.28629(11) 0.01878(19) Uani 1 1 d . . .
H7A H 0.2359 1.0721 0.3657 0.023 Uiso 1 1 calc R . .
C8 C 0.24923(14) 1.20847(11) 0.19344(11) 0.0210(2) Uani 1 1 d . . .
H8A H 0.3259 1.2606 0.2093 0.025 Uiso 1 1 calc R . .
C9 C 0.19079(15) 1.24469(12) 0.07746(11) 0.0239(2) Uani 1 1 d . . .
H9A H 0.2278 1.3212 0.0136 0.029 Uiso 1 1 calc R . .
C10 C 0.07825(15) 1.16899(13) 0.05501(12) 0.0256(2) Uani 1 1 d . . .
H10A H 0.0375 1.1940 -0.0242 0.031 Uiso 1 1 calc R . .
C11 C 0.02472(14) 1.05637(12) 0.14824(11) 0.0217(2) Uani 1 1 d . . .
H11A H -0.0528 1.0052 0.1323 0.026 Uiso 1 1 calc R . .
C12 C 0.08356(12) 1.01798(10) 0.26463(10) 0.01642(18) Uani 1 1 d . . .
C13 C 0.88262(11) 0.30914(10) 0.47503(10) 0.01607(18) Uani 1 1 d . . .
H13A H 0.9458 0.2591 0.4227 0.019 Uiso 1 1 calc R . .
H13B H 0.9457 0.3789 0.4895 0.019 Uiso 1 1 calc R . .
C14 C 0.67408(13) 0.27702(11) 0.30524(11) 0.01844(19) Uani 1 1 d . A .
H14A H 0.5828 0.3146 0.2582 0.022 Uiso 1 1 calc R . .
H14B H 0.7603 0.2710 0.2442 0.022 Uiso 1 1 calc R . .
C15 C 0.64533(15) 0.13074(12) 0.38719(12) 0.0234(2) Uani 1 1 d . . .
H15A H 0.6162 0.0746 0.3360 0.035 Uiso 1 1 calc R A .
H15B H 0.5629 0.1353 0.4503 0.035 Uiso 1 1 calc R . .
H15C H 0.7384 0.0885 0.4279 0.035 Uiso 1 1 calc R . .
C16 C 0.82554(12) 0.52986(11) 0.26864(10) 0.01617(18) Uani 1 1 d . A .
H16A H 0.7540 0.5821 0.2061 0.019 Uiso 1 1 calc R . .
H16B H 0.8603 0.5966 0.3083 0.019 Uiso 1 1 calc R . .
C17 C 0.96413(13) 0.47776(12) 0.19974(12) 0.0224(2) Uani 1 1 d . . .
H17A H 1.0087 0.5565 0.1376 0.034 Uiso 1 1 calc R A .
H17B H 0.9325 0.4124 0.1585 0.034 Uiso 1 1 calc R . .
H17C H 1.0400 0.4310 0.2590 0.034 Uiso 1 1 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
P2 Mo1 P2 180.0 2_666 .
P2 Mo1 P1 86.488(9) 2_666 .
P2 Mo1 P1 93.513(9) . .
P2 Mo1 P1 93.512(9) 2_666 2_666
P2 Mo1 P1 86.487(9) . 2_666
P1 Mo1 P1 180.000(1) . 2_666
P2 Mo1 Br1 86.189(7) 2_666 2_666
P2 Mo1 Br1 93.811(7) . 2_666
P1 Mo1 Br1 85.195(7) . 2_666
P1 Mo1 Br1 94.806(7) 2_666 2_666
P2 Mo1 Br1 93.811(7) 2_666 .
P2 Mo1 Br1 86.189(7) . .
P1 Mo1 Br1 94.805(7) . .
P1 Mo1 Br1 85.195(7) 2_666 .
Br1 Mo1 Br1 179.999(1) 2_666 .
C5 N1 C13 111.74(8) . 2_666
C5 N1 C6 110.55(8) . .
C13 N1 C6 110.73(8) 2_666 .
C1' P1 C5 108.13(14) . .
C1' P1 C3 105.56(16) . .
C5 P1 C3 98.41(5) . .
C1' P1 C1 14.70(11) . .
C5 P1 C1 93.60(9) . .
C3 P1 C1 106.45(10) . .
C1' P1 Mo1 112.10(15) . .
C5 P1 Mo1 115.37(4) . .
C3 P1 Mo1 116.01(4) . .
C1 P1 Mo1 122.45(9) . .
C14 P2 C16 102.81(5) . .
C14 P2 C13 101.84(5) . .
C16 P2 C13 96.86(5) . .
C14 P2 Mo1 117.61(4) . .
C16 P2 Mo1 114.82(3) . .
C13 P2 Mo1 119.64(4) . .
C2 C1 P1 115.32(16) . .
C2 C1 H1B 108.4 . .
P1 C1 H1B 108.4 . .
C2 C1 H1C 108.4 . .
P1 C1 H1C 108.4 . .
H1B C1 H1C 107.5 . .
C2' C1' P1 119.9(3) . .
C2' C1' H1'A 107.4 . .
P1 C1' H1'A 107.4 . .
C2' C1' H1'B 107.4 . .
P1 C1' H1'B 107.4 . .
H1'A C1' H1'B 106.9 . .
C1' C2' H2'A 109.5 . .
C1' C2' H2'B 109.5 . .
H2'A C2' H2'B 109.5 . .
C1' C2' H2'C 109.5 . .
H2'A C2' H2'C 109.5 . .
H2'B C2' H2'C 109.5 . .
C4 C3 P1 120.10(10) . .
C4 C3 H3A 107.3 . .
P1 C3 H3A 107.3 . .
C4 C3 H3B 107.3 . .
P1 C3 H3B 107.3 . .
H3A C3 H3B 106.9 . .
C3 C4 H4A 109.5 . .
C3 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
C3 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
N1 C5 P1 113.01(7) . .
N1 C5 H5A 109.0 . .
P1 C5 H5A 109.0 . .
N1 C5 H5B 109.0 . .
P1 C5 H5B 109.0 . .
H5A C5 H5B 107.8 . .
N1 C6 C12 111.37(9) . .
N1 C6 H6A 109.4 . .
C12 C6 H6A 109.4 . .
N1 C6 H6B 109.4 . .
C12 C6 H6B 109.4 . .
H6A C6 H6B 108.0 . .
C8 C7 C12 120.88(10) . .
C8 C7 H7A 119.6 . .
C12 C7 H7A 119.6 . .
C9 C8 C7 119.99(11) . .
C9 C8 H8A 120.0 . .
C7 C8 H8A 120.0 . .
C10 C9 C8 119.78(11) . .
C10 C9 H9A 120.1 . .
C8 C9 H9A 120.1 . .
C9 C10 C11 120.15(11) . .
C9 C10 H10A 119.9 . .
C11 C10 H10A 119.9 . .
C10 C11 C12 120.66(11) . .
C10 C11 H11A 119.7 . .
C12 C11 H11A 119.7 . .
C11 C12 C7 118.54(10) . .
C11 C12 C6 121.68(10) . .
C7 C12 C6 119.77(10) . .
N1 C13 P2 114.33(7) 2_666 .
N1 C13 H13A 108.7 2_666 .
P2 C13 H13A 108.7 . .
N1 C13 H13B 108.7 2_666 .
P2 C13 H13B 108.7 . .
H13A C13 H13B 107.6 . .
C15 C14 P2 115.14(8) . .
C15 C14 H14A 108.5 . .
P2 C14 H14A 108.5 . .
C15 C14 H14B 108.5 . .
P2 C14 H14B 108.5 . .
H14A C14 H14B 107.5 . .
C14 C15 H15A 109.5 . .
C14 C15 H15B 109.5 . .
H15A C15 H15B 109.5 . .
C14 C15 H15C 109.5 . .
H15A C15 H15C 109.5 . .
H15B C15 H15C 109.5 . .
C17 C16 P2 118.08(8) . .
C17 C16 H16A 107.8 . .
P2 C16 H16A 107.8 . .
C17 C16 H16B 107.8 . .
P2 C16 H16B 107.8 . .
H16A C16 H16B 107.1 . .
C16 C17 H17A 109.5 . .
C16 C17 H17B 109.5 . .
H17A C17 H17B 109.5 . .
C16 C17 H17C 109.5 . .
H17A C17 H17C 109.5 . .
H17B C17 H17C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mo1 P2 2.4981(3) 2_666
Mo1 P2 2.4981(3) .
Mo1 P1 2.4999(3) .
Mo1 P1 2.5000(3) 2_666
Mo1 Br1 2.57771(12) 2_666
Mo1 Br1 2.57773(13) .
N1 C5 1.4625(14) .
N1 C13 1.4632(14) 2_666
N1 C6 1.4748(13) .
P1 C1' 1.810(5) .
P1 C5 1.8441(11) .
P1 C3 1.8503(12) .
P1 C1 1.867(3) .
P2 C14 1.8464(11) .
P2 C16 1.8486(11) .
P2 C13 1.8503(10) .
C1 C2 1.528(3) .
C1 H1B 0.9900 .
C1 H1C 0.9900 .
C2 H2A 0.9800 .
C2 H2B 0.9800 .
C2 H2C 0.9800 .
C1' C2' 1.510(6) .
C1' H1'A 0.9900 .
C1' H1'B 0.9900 .
C2' H2'A 0.9800 .
C2' H2'B 0.9800 .
C2' H2'C 0.9800 .
C3 C4 1.5200(19) .
C3 H3A 0.9900 .
C3 H3B 0.9900 .
C4 H4A 0.9800 .
C4 H4B 0.9800 .
C4 H4C 0.9800 .
C5 H5A 0.9900 .
C5 H5B 0.9900 .
C6 C12 1.5091(15) .
C6 H6A 0.9900 .
C6 H6B 0.9900 .
C7 C8 1.3872(16) .
C7 C12 1.3951(15) .
C7 H7A 0.9500 .
C8 C9 1.3860(17) .
C8 H8A 0.9500 .
C9 C10 1.3849(18) .
C9 H9A 0.9500 .
C10 C11 1.3910(17) .
C10 H10A 0.9500 .
C11 C12 1.3909(16) .
C11 H11A 0.9500 .
C13 N1 1.4632(14) 2_666
C13 H13A 0.9900 .
C13 H13B 0.9900 .
C14 C15 1.5274(16) .
C14 H14A 0.9900 .
C14 H14B 0.9900 .
C15 H15A 0.9800 .
C15 H15B 0.9800 .
C15 H15C 0.9800 .
C16 C17 1.5286(15) .
C16 H16A 0.9900 .
C16 H16B 0.9900 .
C17 H17A 0.9800 .
C17 H17B 0.9800 .
C17 H17C 0.9800 .
