# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
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#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
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#  data retrieval see:
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#  from this site to visualise CIF-encoded structures and 
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data_shelx

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 Mo(CO)4(PH2C(O)NH2)2
;
_contact_author_fax              '+44 1865 272690'
_chemical_name_common            .
_chemical_melting_point          .
_chemical_formula_moiety         'C6 H8 Mo N2 O6 P2'
_chemical_formula_sum            'C6 H8 Mo N2 O6 P2'
_chemical_formula_weight         362.02

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -0.0483 2.7339 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   7.1284(2)
_cell_length_b                   9.7853(2)
_cell_length_c                   18.2084(5)
_cell_angle_alpha                90
_cell_angle_beta                 94.130(2)
_cell_angle_gamma                90
_cell_volume                     1266.80(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    13054
_cell_measurement_theta_min      4.5149
_cell_measurement_theta_max      76.6715

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    .
_exptl_crystal_density_diffrn    1.898
_exptl_crystal_F_000             712
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    11.075
_shelx_estimated_absorpt_T_min   0.306
_shelx_estimated_absorpt_T_max   0.607
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.46062
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.4102
_diffrn_standards_number         .
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_decay_%        .
_diffrn_reflns_number            25541
_diffrn_reflns_av_unetI/netI     0.0126
_diffrn_reflns_av_R_equivalents  0.0316
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         4.870
_diffrn_reflns_theta_max         76.865
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             2649
_reflns_number_gt                2550
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'WinGX (Farrugia, 2005)'
_computing_publication_material  'XCIF (Sheldrick, 2001)'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0314P)²+0.4676P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     .
_atom_sites_solution_secondary   .
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2649
_refine_ls_number_parameters     190
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0193
_refine_ls_R_factor_gt           0.0187
_refine_ls_wR_factor_ref         0.0512
_refine_ls_wR_factor_gt          0.0507
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_restrained_S_all      1.073
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.81074(2) 0.24912(2) 0.18458(2) 0.01764(6) Uani 1 1 d . . . . .
P1 P 1.09256(6) 0.35621(4) 0.13645(2) 0.02272(9) Uani 1 1 d . . . . .
C1 C 1.1970(2) 0.27046(16) 0.05720(10) 0.0220(3) Uani 1 1 d . . . . .
O1 O 1.19552(18) 0.14483(12) 0.05516(7) 0.0307(3) Uani 1 1 d . . . . .
N1 N 1.2674(2) 0.34863(14) 0.00653(8) 0.0305(3) Uani 1 1 d . . . . .
H1A H 1.3169 0.3110 -0.0315 0.037 Uiso 1 1 calc R U . . .
H1B H 1.2645 0.4382 0.0109 0.037 Uiso 1 1 calc R U . . .
P2 P 0.72340(5) 0.13879(4) 0.06432(2) 0.02089(9) Uani 1 1 d . . . . .
C2 C 0.7800(2) 0.23039(16) -0.02154(10) 0.0238(3) Uani 1 1 d . . . . .
O2 O 0.7766(2) 0.35570(13) -0.02160(8) 0.0410(3) Uani 1 1 d . . . . .
N2 N 0.8243(2) 0.15540(15) -0.07855(8) 0.0305(3) Uani 1 1 d . . . . .
H2A H 0.8536 0.1954 -0.1195 0.037 Uiso 1 1 calc R U . . .
H2B H 0.8244 0.0657 -0.0754 0.037 Uiso 1 1 calc R U . . .
C3 C 0.6677(2) 0.42056(16) 0.14914(8) 0.0226(3) Uani 1 1 d . . . . .
O3 O 0.59224(18) 0.51681(12) 0.12764(7) 0.0323(3) Uani 1 1 d . . . . .
C4 C 0.8735(2) 0.32141(16) 0.28592(9) 0.0268(3) Uani 1 1 d . . . . .
O4 O 0.9001(2) 0.35502(15) 0.34612(7) 0.0426(3) Uani 1 1 d . . . . .
C5 C 0.9707(2) 0.07903(16) 0.20646(8) 0.0222(3) Uani 1 1 d . . . . .
O5 O 1.06109(17) -0.01665(12) 0.21454(6) 0.0308(3) Uani 1 1 d . . . . .
C6 C 0.5834(2) 0.17358(17) 0.22789(9) 0.0276(3) Uani 1 1 d . . . . .
O6 O 0.4545(2) 0.13717(15) 0.25678(9) 0.0454(4) Uani 1 1 d . . . . .
H1 H 1.094(3) 0.483(2) 0.1120(14) 0.049(7) Uani 1 1 d . . . . .
H2 H 1.243(3) 0.357(2) 0.1786(13) 0.042(6) Uani 1 1 d . . . . .
H5 H 0.553(3) 0.120(2) 0.0454(13) 0.039(6) Uani 1 1 d . . . . .
H6 H 0.783(3) 0.019(2) 0.0505(12) 0.034(5) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo1 C6 1.9945(16) . ?
Mo1 C4 1.9967(16) . ?
Mo1 C5 2.0406(15) . ?
Mo1 C3 2.0435(16) . ?
Mo1 P2 2.4803(4) . ?
Mo1 P1 2.4811(4) . ?
P1 C1 1.8695(18) . ?
P1 H1 1.32(3) . ?
P1 H2 1.27(2) . ?
C1 O1 1.2299(19) . ?
C1 N1 1.325(2) . ?
N1 H1A 0.8800 . ?
N1 H1B 0.8800 . ?
P2 C2 1.8709(18) . ?
P2 H5 1.25(2) . ?
P2 H6 1.28(2) . ?
C2 O2 1.2264(19) . ?
C2 N2 1.328(2) . ?
N2 H2A 0.8800 . ?
N2 H2B 0.8800 . ?
C3 O3 1.140(2) . ?
C4 O4 1.147(2) . ?
C5 O5 1.140(2) . ?
C6 O6 1.148(2) . ?

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
_geom_angle_publ_flag
C6 Mo1 C4 84.28(7) . . ?
C6 Mo1 C5 94.54(6) . . ?
C4 Mo1 C5 91.35(6) . . ?
C6 Mo1 C3 91.60(6) . . ?
C4 Mo1 C3 94.27(6) . . ?
C5 Mo1 C3 172.06(6) . . ?
C6 Mo1 P2 91.62(5) . . ?
C4 Mo1 P2 174.52(5) . . ?
C5 Mo1 P2 85.33(4) . . ?
C3 Mo1 P2 89.47(4) . . ?
C6 Mo1 P1 176.16(5) . . ?
C4 Mo1 P1 92.49(5) . . ?
C5 Mo1 P1 87.60(4) . . ?
C3 Mo1 P1 86.56(4) . . ?
P2 Mo1 P1 91.725(13) . . ?
C1 P1 Mo1 117.43(5) . . ?
C1 P1 H1 98.7(10) . . ?
Mo1 P1 H1 122.7(10) . . ?
C1 P1 H2 95.9(10) . . ?
Mo1 P1 H2 117.3(10) . . ?
H1 P1 H2 99.9(15) . . ?
O1 C1 N1 123.99(16) . . ?
O1 C1 P1 117.97(13) . . ?
N1 C1 P1 118.04(12) . . ?
C1 N1 H1A 120.0 . . ?
C1 N1 H1B 120.0 . . ?
H1A N1 H1B 120.0 . . ?
C2 P2 Mo1 118.27(5) . . ?
C2 P2 H5 95.9(11) . . ?
Mo1 P2 H5 118.8(11) . . ?
C2 P2 H6 100.3(9) . . ?
Mo1 P2 H6 120.4(10) . . ?
H5 P2 H6 98.4(14) . . ?
O2 C2 N2 123.88(17) . . ?
O2 C2 P2 118.33(14) . . ?
N2 C2 P2 117.79(12) . . ?
C2 N2 H2A 120.0 . . ?
C2 N2 H2B 120.0 . . ?
H2A N2 H2B 120.0 . . ?
O3 C3 Mo1 177.67(13) . . ?
O4 C4 Mo1 174.46(16) . . ?
O5 C5 Mo1 176.16(13) . . ?
O6 C6 Mo1 175.00(17) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1B O2 0.88 2.05 2.9251(19) 173.0 3_765
N1 H1A O3 0.88 2.55 3.0093(18) 113.6 3_765
N2 H2B O1 0.88 2.10 2.9734(19) 172.2 3_755
N2 H2A O5 0.88 2.57 2.9890(18) 110.5 3_755

_refine_diff_density_max         0.335
_refine_diff_density_min         -0.699
_refine_diff_density_rms         0.067

_shelxl_version_number           2014-3


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: dichloromethane'
_chemical_properties_physical    'Air-sensitive, Moisture-sensitive'
_database_code_depnum_ccdc_archive 'CCDC 1014321'
