#------------------------------------------------------------------------------
#$Date: 2017-03-02 19:20:33 +0200 (Thu, 02 Mar 2017) $
#$Revision: 192782 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/11/57/7115759.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_7115759
loop_
_publ_author_name
'M. B. Geeson'
'A. R. Jupp'
'J. E. McGrady'
'J. M. Goicoechea'
_publ_contact_author_fax         '+44 1865 272690'
_publ_section_title
;
 On the coordination chemistry of phosphinecarboxamide: assessing ligand
 basicity
;
_journal_name_full               Chem.Commun.
_journal_page_first              12281
_journal_paper_doi               10.1039/C4cc06094F
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         'C6 H8 Mo N2 O6 P2'
_chemical_formula_sum            'C6 H8 Mo N2 O6 P2'
_chemical_formula_weight         362.02
_chemical_name_systematic
;
 Mo(CO)4(PH2C(O)NH2)2
;
_chemical_properties_physical    'Air-sensitive, Moisture-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 94.130(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.1284(2)
_cell_length_b                   9.7853(2)
_cell_length_c                   18.2084(5)
_cell_measurement_reflns_used    13054
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      76.6715
_cell_measurement_theta_min      4.5149
_cell_volume                     1266.80(6)
_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_collection
;
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_molecular_graphics    'WinGX (Farrugia, 2005)'
_computing_publication_material  'XCIF (Sheldrick, 2001)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.4102
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0316
_diffrn_reflns_av_unetI/netI     0.0126
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            25541
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         76.865
_diffrn_reflns_theta_min         4.870
_exptl_absorpt_coefficient_mu    11.075
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.46062
_exptl_absorpt_correction_type   multi-scan
_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_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.898
_exptl_crystal_description       plate
_exptl_crystal_F_000             712
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane'
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.335
_refine_diff_density_min         -0.699
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         2649
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0193
_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
'w=1/[σ²(Fo²)+(0.0314P)²+0.4676P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0507
_refine_ls_wR_factor_ref         0.0512
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2550
_reflns_number_total             2649
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c4cc06094f2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
;
The following automatic conversions were performed:
data name '_contact_author_fax' replaced with
'_publ_contact_author_fax' as specified in the replacement file
'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 4998 2017-03-02 13:24:31Z antanas 
;
_cod_database_code               7115759
#BEGIN Tags that were not found in dictionaries:
_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.
;
_shelx_estimated_absorpt_t_min   0.306
_shelx_estimated_absorpt_t_max   0.607
_shelxl_version_number           2014-3
#END Tags that were not found in dictionaries
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'
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
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 . .
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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
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_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
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_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
