# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_alphaCuPhP
_database_code_depnum_ccdc_archive 'CCDC 1490687'
_audit_update_record             
;
2016-07-05 deposited with the CCDC.
2016-10-06 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT043_alphaCuPhP          
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..       7.06 Check
RESPONSE: Hydrogen atoms were not inserted but given in the sum formula.
;
_vrf_PLAT049_alphaCuPhP          
;
PROBLEM: Calculated Density less than 1.0 gcm-3 .........     0.9837 Check
RESPONSE: Hydrogen atoms were not inserted but given in the sum formula.
;
# Added during the CSD deposition process: Tuesday 05 July 2016 02:41 PM
# end Validation Reply Form

_chemical_name_mineral           alphaCuPhP
_cell_length_a                   5.65908(15)
_cell_length_b                   14.3406(5)
_cell_length_c                   4.79644(13)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     389.25(2)
_cell_formula_units_Z            1
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P m n 21'
_symmetry_Int_Tables_number      31
_space_group_name_Hall           'P 2ac -2'
_cell_measurement_temperature    293
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z '
'-x+1/2, -y, z+1/2 '
'-x, y, z '
'x+1/2, -y, z+1/2 '
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_B_iso_or_equiv
Cu1 Cu 2 1 0.48322 -0.1569298 0.5 3
P1 P 2 1 0.6195274 0.3835084 0.5 3
O1 O 2 1 0.6034(12) 0.055(3) 0.5 3
O2 O 4 0.8030(16) 0.5788(7) 0.573(2) 0.5 3
O3 O 2 1 0.3726(11) -0.488(3) 0.5 3
C1 C 2 1 0.7523 0.4371 0.5 3
C2 C 2 1 0.8111 0.2189 0.25 3
C3 C 2 1 0.9068 0.2592 0.25 3
C4 C 2 1 0.9499 0.5119 0.5 3
C5 C 2 1 0.8892 0.7309 0.25 3
C6 C 2 1 0.7935 0.6971 0.25 3
C2A C 4 0.7786 0.802 0.4175 0.25 3
C3A C 4 0.7669 0.8935 0.4603 0.25 3


_geom_special_details            
;
 Bond distances, angles etc. have been calculated using the
 rounded fractional coordinates. All su's are estimated
 from the variances of the (full) variance-covariance matrix.
 The cell esds are taken into account in the estimation of
 distances, angles and torsion angles
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O1 2.001(17) . . yes
Cu1 O3 2.245(15) . . yes
Cu1 P1 2.9461(1) . 1_554 yes
Cu1 O2 2.191(10) . 1_554 yes
P1 O1 1.593(14) . . yes
P1 O2 1.552(9) . . yes
P1 C1 1.9213(1) . . yes
P1 O2 1.552(9) . 3_755 yes
C1 C2 1.3440(1) . . no
C1 C2A 1.4445 . . no
C1 C6 1.3800(1) . . no
C1 C2A 1.4445 . 3_755 no
C2 C2A 1.5793 . . no
C2 C3 1.3859(1) . . no
C2 C2A 1.5793 . 3_755 no
C2A C3A 1.3298 . . no
C3 C3A 1.6453 . . no
C3 C3A 1.6453 . 3_755 no
C5 C6 1.3819(1) . . no

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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Cu1 O3 165.5(6) . . . yes
P1 Cu1 O1 79.0(4) 1_554 . . yes
O1 Cu1 O2 76.2(4) . . 1_554 yes
P1 Cu1 O3 86.5(4) 1_554 . . yes
O2 Cu1 O3 91.4(4) 1_554 . . yes
P1 Cu1 O2 31.0(2) 1_554 . 1_554 yes
O1 P1 O2 121.6(5) . . . yes
O1 P1 C1 106.0(6) . . . yes
Cu1 P1 O1 130.1(6) 1_556 . . yes
O1 P1 O2 121.6(5) . . 3_755 yes
O2 P1 C1 107.1(4) . . . yes
Cu1 P1 O2 46.6(4) 1_556 . . yes
O2 P1 O2 91.8(5) . . 3_755 yes
Cu1 P1 C1 123.88 1_556 . . yes
O2 P1 C1 107.1(4) 3_755 . . yes
Cu1 P1 O2 46.6(3) 1_556 . 3_755 yes
Cu1 O1 P1 128.9(10) . . . yes
C2A C2 C3 89.87 . . . no
C2A C2 C2A 105.00 . . 3_755 no
C2A C2 C3 89.87 3_755 . . no
C2 C2A C3A 92.93 . . . no
C2 C3 C3A 88.11 . . . no
C2 C3 C3A 88.11 . . 3_755 no
C3A C3 C3A 106.60 . . 3_755 no
C2A C3A C3 89.08 . . . no

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 P1 O1 Cu1 -57.5(5) . . . . no
C1 P1 O1 Cu1 180.00 . . . . no



_chemical_name_common            'Copper(II)-phenylphosphonate monohydrate'
_chemical_formula_moiety         'C6 H7 Cu O4 P'
_chemical_formula_sum            'C6 H7 Cu O4 P'
_chemical_formula_weight         237.64
_chemical_compound_source        'mechanochemical synthesis'
_exptl_crystal_description       block
_exptl_crystal_colour            'pale turquoise'
_diffrn_ambient_temperature      293
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_measurement_device_type  'insertion device'
_diffrn_radiation_wavelength     1.5406
_exptl_crystal_density_diffrn    1.014
_exptl_crystal_density_method    'Not Measured'


_pd_meas_2theta_range_min        4
_pd_meas_2theta_range_max        60



_diffrn_radiation_monochromator  none
_cell_measurement_reflns_used    25
_cell_measurement_theta_min      2
_cell_measurement_theta_max      20


_pd_proc_2theta_range_inc        0.009
_pd_proc_info_excluded_regions   none
_pd_proc_ls_background_function  ?
_pd_proc_number_of_points        21236
_pd_spec_mount_mode              transmission
_pd_spec_mounting                '0.5 mm glass capillary'
_pd_spec_shape                   cylinder
_pd_spec_size_axial              10
_pd_spec_size_equat              0.5
_pd_spec_size_thick              0.5
_pd_proc_ls_prof_wR_factor       10.46
_refine_ls_goodness_of_fit_all   8.91
_refine_ls_R_I_factor            8.225
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_mws029t
_database_code_depnum_ccdc_archive 'CCDC 1490688'
_audit_update_record             
;
2016-10-04 deposited with the CCDC.
2016-10-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        'Copper Phenylphosphonate'
_chemical_name_common            'Copper Phenylphosphonate'
_chemical_melting_point          ?
_chemical_formula_moiety         'C6 H7 Cu O4 P'
_chemical_formula_sum            'C6 H7 Cu O4 P'
_chemical_formula_weight         237.63

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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   13.9871(7)
_cell_length_b                   7.6637(4)
_cell_length_c                   7.4534(4)
_cell_angle_alpha                90
_cell_angle_beta                 91.750(2)
_cell_angle_gamma                90
_cell_volume                     798.58(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    321
_cell_measurement_theta_min      2
_cell_measurement_theta_max      20
_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.976
_exptl_crystal_F_000             476

_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_exptl_absorpt_coefficient_mu    2.902
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_correction_T_min  0.25
_exptl_absorpt_correction_T_max  0.4
_exptl_absorpt_process_details   'SHELXTL (Bruker, 2001)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      180(2)
_diffrn_radiation_wavelength     0.71073

_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX CCD area-detector'
_diffrn_measurement_method       ω/2θ

_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            18199
_diffrn_reflns_av_unetI/netI     0.0415
_diffrn_reflns_av_R_equivalents  0.1235
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         2.914
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             1828
_reflns_number_gt                1757
_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      'SMART (Bruker, 2001)'
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    
'SHELXTL (Bruker, 2001), ORTEPIII (Burnett & Johnson, 1996)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_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)+(0.0323P)²+1.3387P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.0099(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1828
_refine_ls_number_parameters     110
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0330
_refine_ls_R_factor_gt           0.0318
_refine_ls_wR_factor_ref         0.0829
_refine_ls_wR_factor_gt          0.0820
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_restrained_S_all      5.748
_refine_ls_shift/su_max          0.000
_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
Cu1 Cu -0.02278(2) 0.19130(3) 0.05605(3) 0.00792(14) Uani 1 1 d . . . . .
P1 P 0.11157(4) 0.04510(7) 0.35175(7) 0.00697(16) Uani 1 1 d . . . . .
O1 O 0.05620(11) 0.0096(2) 0.1744(2) 0.0095(3) Uani 1 1 d . . . . .
O2 O 0.08870(12) 0.2262(2) 0.4262(2) 0.0107(3) Uani 1 1 d . . . . .
O3 O 0.09457(11) -0.0982(2) 0.4896(2) 0.0098(3) Uani 1 1 d D . . . .
H1 H -0.1289 -0.0321 0.1207 0.015 Uiso 1 1 d DR U . . .
H2 H -0.1302 0.0984 0.2754 0.015 Uiso 1 1 d DR U . . .
O4 O -0.13719(13) 0.0783(2) 0.1585(2) 0.0144(4) Uani 1 1 d . . . . .
C1 C 0.23774(16) 0.0381(3) 0.3096(3) 0.0118(4) Uani 1 1 d . . . . .
C2 C 0.27731(19) 0.1492(4) 0.1844(4) 0.0223(6) Uani 1 1 d . . . . .
H3 H 0.2386 0.2309 0.1251 0.027 Uiso 1 1 calc R U . . .
C3 C 0.3738(2) 0.1400(5) 0.1468(4) 0.0308(7) Uani 1 1 d . . . . .
H4 H 0.3993 0.2151 0.0627 0.037 Uiso 1 1 calc R U . . .
C4 C 0.4322(2) 0.0188(5) 0.2343(5) 0.0320(7) Uani 1 1 d . . . . .
H5 H 0.4967 0.0112 0.2083 0.038 Uiso 1 1 calc R U . . .
C5 C 0.3935(2) -0.0908(5) 0.3610(5) 0.0387(8) Uani 1 1 d . . . . .
H6 H 0.4327 -0.1703 0.4223 0.046 Uiso 1 1 calc R U . . .
C6 C 0.2968(2) -0.0831(4) 0.3971(5) 0.0295(7) Uani 1 1 d . . . . .
H7 H 0.2714 -0.1592 0.4803 0.035 Uiso 1 1 calc R U . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu1 0.00869(18) 0.00660(19) 0.00875(18) 0.00096(9) 0.00481(11) 0.00020(8)
P1 0.0067(3) 0.0065(3) 0.0080(3) 0.00020(19) 0.00410(19) 0.00044(18)
O1 0.0121(7) 0.0078(7) 0.0088(7) 0.0000(6) 0.0033(6) 0.0006(6)
O2 0.0101(8) 0.0077(7) 0.0147(8) -0.0020(6) 0.0064(6) 0.0002(6)
O3 0.0111(8) 0.0085(7) 0.0101(7) 0.0024(6) 0.0026(6) -0.0008(6)
O4 0.0162(8) 0.0144(8) 0.0130(8) -0.0010(6) 0.0071(6) -0.0011(7)
C1 0.0091(10) 0.0131(11) 0.0135(10) -0.0025(8) 0.0048(8) 0.0008(8)
C2 0.0122(11) 0.0339(15) 0.0211(12) 0.0118(12) 0.0038(9) -0.0027(11)
C3 0.0152(13) 0.050(2) 0.0272(14) 0.0112(14) 0.0092(11) -0.0060(13)
C4 0.0100(12) 0.0449(18) 0.0417(17) -0.0005(15) 0.0110(11) 0.0022(12)
C5 0.0160(14) 0.0374(18) 0.063(2) 0.0168(17) 0.0104(14) 0.0118(13)
C6 0.0168(13) 0.0271(15) 0.0454(17) 0.0180(13) 0.0109(12) 0.0065(11)

_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
Cu1 O3 1.9248(16) 2 ?
Cu1 O2 1.9644(16) 4_565 ?
Cu1 O1 1.9694(16) . ?
Cu1 O4 1.9922(17) . ?
Cu1 O1 2.3432(15) 3 ?
P1 O3 1.5276(16) . ?
P1 O2 1.5324(17) . ?
P1 O1 1.5357(16) . ?
P1 C1 1.803(2) . ?
O1 Cu1 2.3432(15) 3 ?
O2 Cu1 1.9644(16) 4_566 ?
O3 Cu1 1.9247(16) 2_545 ?
O4 H1 0.9000 . ?
O4 H2 0.8876 . ?
C1 C2 1.391(3) . ?
C1 C6 1.392(4) . ?
C2 C3 1.389(4) . ?
C2 H3 0.9300 . ?
C3 C4 1.386(5) . ?
C3 H4 0.9300 . ?
C4 C5 1.386(5) . ?
C4 H5 0.9300 . ?
C5 C6 1.389(4) . ?
C5 H6 0.9300 . ?
C6 H7 0.9300 . ?

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
O3 Cu1 O2 93.50(7) 2 4_565 ?
O3 Cu1 O1 162.59(7) 2 . ?
O2 Cu1 O1 90.31(7) 4_565 . ?
O3 Cu1 O4 90.64(7) 2 . ?
O2 Cu1 O4 170.97(7) 4_565 . ?
O1 Cu1 O4 88.11(7) . . ?
O3 Cu1 O1 109.25(6) 2 3 ?
O2 Cu1 O1 89.65(6) 4_565 3 ?
O1 Cu1 O1 87.74(6) . 3 ?
O4 Cu1 O1 81.41(6) . 3 ?
O3 P1 O2 111.67(9) . . ?
O3 P1 O1 111.50(9) . . ?
O2 P1 O1 111.53(9) . . ?
O3 P1 C1 105.61(10) . . ?
O2 P1 C1 107.85(10) . . ?
O1 P1 C1 108.38(10) . . ?
P1 O1 Cu1 121.43(9) . . ?
P1 O1 Cu1 146.25(10) . 3 ?
Cu1 O1 Cu1 92.26(6) . 3 ?
P1 O2 Cu1 130.35(10) . 4_566 ?
P1 O3 Cu1 125.09(9) . 2_545 ?
Cu1 O4 H1 100.1 . . ?
Cu1 O4 H2 103.6 . . ?
H1 O4 H2 117.3 . . ?
C2 C1 C6 118.7(2) . . ?
C2 C1 P1 120.70(19) . . ?
C6 C1 P1 120.56(19) . . ?
C3 C2 C1 120.9(3) . . ?
C3 C2 H3 119.6 . . ?
C1 C2 H3 119.6 . . ?
C4 C3 C2 120.1(3) . . ?
C4 C3 H4 120.0 . . ?
C2 C3 H4 120.0 . . ?
C5 C4 C3 119.4(3) . . ?
C5 C4 H5 120.3 . . ?
C3 C4 H5 120.3 . . ?
C4 C5 C6 120.6(3) . . ?
C4 C5 H6 119.7 . . ?
C6 C5 H6 119.7 . . ?
C5 C6 C1 120.4(3) . . ?
C5 C6 H7 119.8 . . ?
C1 C6 H7 119.8 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O3 P1 O1 Cu1 131.11(10) . . . . ?
O2 P1 O1 Cu1 5.51(14) . . . . ?
C1 P1 O1 Cu1 -113.06(12) . . . . ?
O3 P1 O1 Cu1 -52.32(19) . . . 3 ?
O2 P1 O1 Cu1 -177.92(15) . . . 3 ?
C1 P1 O1 Cu1 63.50(19) . . . 3 ?
O3 P1 O2 Cu1 -47.20(16) . . . 4_566 ?
O1 P1 O2 Cu1 78.30(15) . . . 4_566 ?
C1 P1 O2 Cu1 -162.81(13) . . . 4_566 ?
O2 P1 O3 Cu1 130.83(11) . . . 2_545 ?
O1 P1 O3 Cu1 5.31(14) . . . 2_545 ?
C1 P1 O3 Cu1 -112.20(12) . . . 2_545 ?
O3 P1 C1 C2 177.9(2) . . . . ?
O2 P1 C1 C2 -62.6(2) . . . . ?
O1 P1 C1 C2 58.3(2) . . . . ?
O3 P1 C1 C6 0.2(3) . . . . ?
O2 P1 C1 C6 119.7(2) . . . . ?
O1 P1 C1 C6 -119.4(2) . . . . ?
C6 C1 C2 C3 0.1(4) . . . . ?
P1 C1 C2 C3 -177.7(2) . . . . ?
C1 C2 C3 C4 0.0(5) . . . . ?
C2 C3 C4 C5 -0.8(5) . . . . ?
C3 C4 C5 C6 1.6(6) . . . . ?
C4 C5 C6 C1 -1.5(6) . . . . ?
C2 C1 C6 C5 0.7(5) . . . . ?
P1 C1 C6 C5 178.4(3) . . . . ?

_refine_diff_density_max         0.838
_refine_diff_density_min         -0.621
_refine_diff_density_rms         0.122

_shelx_res_file                  
;

    mws029t.res created by SHELXL-2014/7

TITL MWS029 tidy
CELL  0.71073   13.9871    7.6637    7.4534    90.000    91.750    90.000
ZERR        4    0.0007    0.0004    0.0004     0.000     0.002     0.000
LATT   1
SYMM             - X ,    0.50000 + Y ,    0.50000 - Z
SFAC  C  H Cu  O  P
UNIT    24   28   4  16   4
L.S. 15
FMAP 2
PLAN 20
ACTA
BOND $H
OMIt 0 55
CONF
DFIX 0.9 0.02 O3 H1 O3 H2
DANG 1.7 0.01 H1 H2

WGHT    0.032300    1.338700
EXTI    0.009856
FVAR       0.25867
CU1   3   -0.022775    0.191297    0.056046    11.00000    0.00869    0.00660 =
         0.00875    0.00096    0.00481    0.00020
P1    5    0.111574    0.045101    0.351755    11.00000    0.00665    0.00646 =
         0.00803    0.00020    0.00410    0.00044
O1    4    0.056197    0.009584    0.174428    11.00000    0.01206    0.00784 =
         0.00884   -0.00003    0.00334    0.00058
O2    4    0.088701    0.226235    0.426235    11.00000    0.01007    0.00769 =
         0.01475   -0.00197    0.00638    0.00021
O3    4    0.094574   -0.098248    0.489580    11.00000    0.01111    0.00849 =
         0.01008    0.00238    0.00259   -0.00083
AFIX   3
H1    2   -0.128896   -0.032097    0.120703    11.00000   -1.50000
H2    2   -0.130196    0.098403    0.275402    11.00000   -1.50000
AFIX   0

O4    4   -0.137192    0.078265    0.158459    11.00000    0.01617    0.01435 =
         0.01302   -0.00102    0.00705   -0.00108
C1    1    0.237739    0.038068    0.309572    11.00000    0.00907    0.01309 =
         0.01353   -0.00246    0.00478    0.00078
C2    1    0.277308    0.149224    0.184432    11.00000    0.01216    0.03388 =
         0.02108    0.01177    0.00384   -0.00266
AFIX  43
H3    2    0.238626    0.230866    0.125141    11.00000   -1.20000
AFIX   0
C3    1    0.373802    0.139985    0.146782    11.00000    0.01524    0.05036 =
         0.02722    0.01122    0.00920   -0.00600
AFIX  43
H4    2    0.399293    0.215147    0.062743    11.00000   -1.20000
AFIX   0
C4    1    0.432175    0.018833    0.234343    11.00000    0.00995    0.04491 =
         0.04167   -0.00051    0.01096    0.00224
AFIX  43
H5    2    0.496651    0.011239    0.208346    11.00000   -1.20000
AFIX   0
C5    1    0.393542   -0.090841    0.360968    11.00000    0.01600    0.03738 =
         0.06330    0.01684    0.01041    0.01183
AFIX  43
H6    2    0.432721   -0.170332    0.422271    11.00000   -1.20000
AFIX   0
C6    1    0.296815   -0.083060    0.397104    11.00000    0.01678    0.02709 =
         0.04538    0.01798    0.01087    0.00654
AFIX  43
H7    2    0.271372   -0.159216    0.480260    11.00000   -1.20000
AFIX   0
HKLF 4

REM  MWS029 tidy
REM R1 =  0.0318 for    1757 Fo > 4sig(Fo)  and  0.0330 for all    1828 data
REM    110 parameters refined using      3 restraints

END

WGHT      0.0299      1.6090

REM Highest difference peak  0.838,  deepest hole -0.621,  1-sigma level  0.122
Q1    1   0.1797  0.0416  0.3264  11.00000  0.05    0.84
Q2    1  -0.0887  0.2150  0.1012  11.00000  0.05    0.73
Q3    1   0.0393  0.1878  0.0188  11.00000  0.05    0.69
Q4    1   0.1011 -0.1045  0.3961  11.00000  0.05    0.51
Q5    1  -0.0339  0.1841 -0.0533  11.00000  0.05    0.49
Q6    1  -0.0343 -0.0599  0.0805  11.00000  0.05    0.44
Q7    1  -0.0109  0.1946  0.1657  11.00000  0.05    0.44
Q8    1  -0.0836  0.1227  0.1417  11.00000  0.05    0.43
Q9    1  -0.1357  0.1864  0.0464  11.00000  0.05    0.43
Q10   1  -0.2027  0.0405  0.2146  11.00000  0.05    0.42
Q11   1   0.3400 -0.0829  0.3463  11.00000  0.05    0.42
Q12   1   0.0756 -0.1775  0.4913  11.00000  0.05    0.41
Q13   1   0.0880  0.0199  0.2550  11.00000  0.05    0.40
Q14   1   0.2552  0.1141  0.2716  11.00000  0.05    0.40
Q15   1  -0.0246  0.0684  0.0789  11.00000  0.05    0.39
Q16   1   0.3962 -0.0539  0.2595  11.00000  0.05    0.38
Q17   1   0.2755 -0.0596  0.3153  11.00000  0.05    0.38
Q18   1  -0.1975  0.1188  0.1161  11.00000  0.05    0.38
Q19   1  -0.0572  0.0535 -0.0024  11.00000  0.05    0.37
Q20   1   0.0633  0.1685  0.5493  11.00000  0.05    0.34
;
_shelx_res_checksum              67772
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_CuPhP2
_database_code_depnum_ccdc_archive 'CCDC 1490689'
_audit_update_record             
;
2016-07-05 deposited with the CCDC.
2016-10-06 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT411_CuPhP2              
;
PROBLEM: Short Inter H...H Contact  H4A    ..  H4A     ..       1.62 Ang.
RESPONSE: The sructure solution was performed from Powder XRD and the H-atoms were insered manually.
;
_vrf_PLAT780_CuPhP2              
;
PROBLEM: Coordinates do not Form a Properly Connected Set     Please Do !
RESPONSE: Will be completed.
;
# Added during the CSD deposition process: Tuesday 05 July 2016 02:41 PM
# end Validation Reply Form

_chemical_name_mineral           CuPhP2
_cell_length_a                   31.6115(3)
_cell_length_b                   6.08670(6)
_cell_length_c                   7.62568(7)
_cell_angle_alpha                90
_cell_angle_beta                 97.5312(10)
_cell_angle_gamma                90
_cell_volume                     1454.60(2)
_cell_formula_units_Z            4
_symmetry_cell_setting           monoclinic
_space_group                     C12/c1
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_int_tables_number      15
_cell_measurement_temperature    293

loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -x,y,1/2-z
3 -x,-y,-z
4 x,-y,1/2+z
5 1/2+x,1/2+y,z
6 1/2-x,1/2+y,1/2-z
7 1/2-x,1/2-y,-z
8 1/2+x,1/2-y,1/2+z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_B_iso_or_equiv
_atom_site_U_iso_or_equiv

Cu1 Cu 4 0 0 0 1 2.19(4) 0.02774
P1 P 8 0.93485(4) 0.3125(2) 0.66548(15) 1 2.19(4) 0.02774
O1 O 8 0.94159(8) 0.5571(3) 0.6245(3) 1 2.19(4) 0.02774
H1A H 8 0.928968 0.619717 0.509162 1 3 3
O2 O 8 0.95843(9) 0.2721(4) 0.8527(2) 1 2.19(4) 0.02774
O3 O 8 0.94786(9) 0.1536(4) 0.5300(3) 1 2.19(4) 0.02774
C1 C 8 0.87913(5) 0.2747(2) 0.67705(14) 1 2.19(4) 0.02774
C2 C 8 0.84978(4) 0.4293(2) 0.61210(15) 1 2.19(4) 0.02774
H2 H 8 0.85837(9) 0.5578(3) 0.5600(2) 1 2.63(5) 0.03329
C3 C 8 0.80604(5) 0.3918(2) 0.62540(15) 1 2.19(4) 0.02774
H3 H 8 0.78606(9) 0.4967(4) 0.5812(2) 1 2.63(5) 0.03329
C4 C 8 0.79224(5) 0.2041(2) 0.70170(15) 1 2.19(4) 0.02774
H4 H 8 0.76347(8) 0.1820(4) 0.7091(2) 1 2.63(5) 0.03329
C5 C 8 0.82135(5) 0.0528(2) 0.76539(15) 1 2.19(4) 0.02774
H5 H 8 0.81259(9) -0.0754(4) 0.8173(2) 1 2.63(5) 0.03329
C6 C 8 0.86480(5) 0.08554(19) 0.75409(14) 1 2.19(4) 0.02774
H6 H 8 0.88445(8) -0.0211(4) 0.7988(2) 1 2.63(5) 0.03329
O4 O 4 0 0.1777(6) 0.25 1 2.19(4) 0.02774
H4A H 8 0.974129 0.27189 1.23594 1 3 3



_geom_special_details            
;
 Bond distances, angles etc. have been calculated using the
 rounded fractional coordinates. All su's are estimated
 from the variances of the (full) variance-covariance matrix.
 The cell esds are taken into account in the estimation of
 distances, angles and torsion angles
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O4 2.1919(18) . . yes
Cu1 O2 2.312(2) . 1_454 yes
Cu1 O3 1.934(3) . 2_655 yes
Cu1 O4 2.1919(18) . 3_555 yes
Cu1 O2 2.312(2) . 3_656 yes
Cu1 O3 1.934(3) . 4_454 yes
P1 O1 1.542(2) . . yes
P1 O2 1.541(2) . . yes
P1 O3 1.511(3) . . yes
P1 C1 1.790(2) . . yes
O1 H1A 0.9900 . . no
O4 H4A 0.9900 . 2_656 no
O4 H4A 0.9900 . 1_454 no
C1 C6 1.3949(17) . . no
C1 C2 1.3679(18) . . no
C2 C3 1.418(2) . . no
C3 C4 1.3786(18) . . no
C4 C5 1.3467(19) . . no
C5 C6 1.402(2) . . no
C2 H2 0.934(2) . . no
C3 H3 0.930(3) . . no
C4 H4 0.928(3) . . no
C5 H5 0.933(3) . . no
C6 H6 0.932(3) . . no

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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Cu1 O4 90.25(8) 1_454 . . yes
O3 Cu1 O4 87.79(8) 2_655 . . yes
O4 Cu1 O4 180.00 . . 3_555 yes
O2 Cu1 O4 89.75(8) 3_656 . . yes
O3 Cu1 O4 92.21(8) 4_454 . . yes
O2 Cu1 O3 92.02(10) 1_454 . 2_655 yes
O2 Cu1 O4 89.75(8) 1_454 . 3_555 yes
O2 Cu1 O2 180.00 1_454 . 3_656 yes
O2 Cu1 O3 87.98(10) 1_454 . 4_454 yes
O3 Cu1 O4 92.21(8) 2_655 . 3_555 yes
O2 Cu1 O3 87.98(10) 3_656 . 2_655 yes
O3 Cu1 O3 180.00 2_655 . 4_454 yes
O2 Cu1 O4 90.25(8) 3_656 . 3_555 yes
O3 Cu1 O4 87.79(8) 4_454 . 3_555 yes
O2 Cu1 O3 92.02(10) 3_656 . 4_454 yes
O1 P1 O2 106.20(14) . . . yes
O1 P1 O3 114.98(15) . . . yes
O1 P1 C1 107.29(12) . . . yes
O2 P1 O3 112.91(15) . . . yes
O2 P1 C1 107.06(13) . . . yes
O3 P1 C1 108.01(13) . . . yes
Cu1 O2 P1 137.69(14) 1_656 . . yes
Cu1 O3 P1 134.64(17) 2_655 . . yes
Cu1 O4 Cu1 120.86(17) . . 2_555 yes
P1 O1 H1A 120.00 . . . no
Cu1 O4 H4A 107.00 . . 2_656 no
Cu1 O4 H4A 107.00 . . 1_454 no
Cu1 O4 H4A 107.00 2_555 . 2_656 no
Cu1 O4 H4A 107.00 2_555 . 1_454 no
H4A O4 H4A 109.00 1_454 . 2_656 no
P1 C1 C2 121.26(10) . . . yes
P1 C1 C6 120.19(11) . . . yes
C2 C1 C6 118.56(14) . . . no
C1 C2 C3 119.00(12) . . . no
C2 C3 C4 121.94(13) . . . no
C3 C4 C5 118.68(14) . . . no
C4 C5 C6 120.62(12) . . . no
C1 C6 C5 121.21(12) . . . no
C1 C2 H2 120.6(2) . . . no
C3 C2 H2 120.4(2) . . . no
C2 C3 H3 119.1(2) . . . no
C4 C3 H3 119.0(2) . . . no
C3 C4 H4 120.8(2) . . . no
C5 C4 H4 120.50(19) . . . no
C4 C5 H5 119.9(2) . . . no
C6 C5 H5 119.5(2) . . . no
C1 C6 H6 119.4(2) . . . no
C5 C6 H6 119.35(19) . . . no

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 P1 O2 Cu1 -140.6(2) . . . 1_656 no
O3 P1 O2 Cu1 -13.7(3) . . . 1_656 no
C1 P1 O2 Cu1 105.1(2) . . . 1_656 no
O1 P1 O3 Cu1 90.3(2) . . . 2_655 no
O2 P1 O3 Cu1 -31.8(3) . . . 2_655 no
C1 P1 O3 Cu1 -149.95(18) . . . 2_655 no
O1 P1 C1 C2 15.48(16) . . . . no
O1 P1 C1 C6 -164.20(12) . . . . no
O2 P1 C1 C2 129.12(14) . . . . no
O2 P1 C1 C6 -50.55(15) . . . . no
O3 P1 C1 C2 -109.01(14) . . . . no
O3 P1 C1 C6 71.32(15) . . . . no
P1 C1 C2 C3 -179.68(10) . . . . no
C6 C1 C2 C3 0.00(16) . . . . no
P1 C1 C6 C5 179.70(10) . . . . no
C2 C1 C6 C5 0.02(17) . . . . no
C1 C2 C3 C4 -0.06(18) . . . . no
C2 C3 C4 C5 0.09(19) . . . . no
C3 C4 C5 C6 -0.07(18) . . . . no
C4 C5 C6 C1 0.03(18) . . . . no

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
_geom_hbond_publ_flag
#
#D   H   A   D - H  H...A   D...A    D - H...A  symm(A)
#
O1 H1A O2 0.9900 1.7400 2.439(3) 124.00 4_564 yes
O4_b H4A O1 0.9900 1.6200 2.543(3) 152.00 4_565 yes





_chemical_name_common            Copper(II)-bis(phenylphosphonate)_Monohydrate
_chemical_formula_moiety         'C12 H14 Cu O7 P2'
_chemical_formula_sum            'C12 H14 Cu O7 P2'
_chemical_formula_weight         395.73
_chemical_compound_source        'mechanochemical synthesis'
_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_diffrn_ambient_temperature      293
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_measurement_device_type  'D8 Discover, Bruker AXS'
_diffrn_radiation_wavelength     1.5406
_exptl_crystal_density_diffrn    1.807
_exptl_crystal_density_method    'Not Measured'

_diffrn_radiation_monochromator  none
_cell_measurement_reflns_used    25
_cell_measurement_theta_min      2
_cell_measurement_theta_max      20

_pd_meas_2theta_range_min        4
_pd_meas_2theta_range_max        60
_pd_meas_2theta_range_inc        0.009
_pd_proc_info_excluded_regions   none
_pd_proc_ls_background_function  ?
_pd_proc_number_of_points        6222
_pd_spec_mount_mode              transmission
_pd_spec_mounting                '0.5 mm glass capillary'
_pd_spec_shape                   cylinder
_pd_spec_size_axial              10
_pd_spec_size_equat              0.5
_pd_spec_size_thick              0.5
_pd_proc_ls_prof_wR_factor       3.29
_refine_ls_goodness_of_fit_all   2.98
_refine_ls_R_I_factor            6.62
