#------------------------------------------------------------------------------
#$Date: 2024-06-18 00:43:21 +0200 (Tue 18 de Jun de 2024) $
#$Revision: 292435 $
#$URL: svn://www.crystallography.net/cod/cif/7/24/88/7248881.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_7248881
loop_
_publ_author_name
'Ward, Jas S.'
'Kruger, Paul'
_publ_section_title
;
 A Pentametallic Co5L4 Architecture Constructed From Bis-substituted
 Phosphate-based Ligands
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D4CE00468J
_journal_year                    2024
_chemical_formula_moiety         'C12 H13 N2 O4 P'
_chemical_formula_sum            'C12 H13 N2 O4 P'
_chemical_formula_weight         280.21
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2024-05-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2024-06-11 deposited with the CCDC.	2024-06-17 downloaded from the CCDC.
;
_cell_angle_alpha                83.62(3)
_cell_angle_beta                 81.85(3)
_cell_angle_gamma                77.85(3)
_cell_formula_units_Z            2
_cell_length_a                   6.9800(14)
_cell_length_b                   9.0400(18)
_cell_length_c                   10.340(2)
_cell_measurement_reflns_used    436
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.0
_cell_measurement_theta_min      0.4
_cell_volume                     629.2(2)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'φ scans'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_source         'MX1 Beamline Australian Synchrotron'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0527
_diffrn_reflns_av_unetI/netI     0.0417
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            11100
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.373
_diffrn_reflns_theta_min         1.997
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.231
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.479
_exptl_crystal_description       plate
_exptl_crystal_F_000             292
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: methanol/diethylether'
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.257
_refine_diff_density_min         -0.396
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     192
_refine_ls_number_reflns         2560
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0399
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0531P)²+0.3561P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1037
_refine_ls_wR_factor_ref         0.1072
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2265
_reflns_number_total             2560
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4ce00468j2.cif
_cod_data_source_block           Pro_ligand
_cod_database_code               7248881
_shelxl_version_number           2014/6
_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.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C112(H112), C114(H114), C115(H115), C116(H116), C212(H212), C214(H214),
 C215(H215), C216(H216)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_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_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
P1 P 0.79175(6) 0.20259(5) 0.80352(4) 0.01994(15) Uani 1 1 d . . . . .
O11 O 0.70745(18) 0.36928(14) 0.85277(13) 0.0248(3) Uani 1 1 d . . . . .
O12 O 0.8205(2) 0.22677(16) 0.64749(13) 0.0285(3) Uani 1 1 d . . . . .
O13 O 0.63058(18) 0.11778(14) 0.85173(12) 0.0230(3) Uani 1 1 d . . . . .
O14 O 0.99129(19) 0.14044(15) 0.84051(13) 0.0269(3) Uani 1 1 d . . . . .
N117 N 0.7431(2) 0.84591(17) 1.00250(16) 0.0222(3) Uani 1 1 d . . . . .
H11A H 0.831(4) 0.853(3) 1.056(2) 0.031(6) Uiso 1 1 d . . . . .
H11B H 0.628(4) 0.837(3) 1.048(2) 0.031(6) Uiso 1 1 d . . . . .
H11C H 0.713(4) 0.938(3) 0.953(3) 0.041(7) Uiso 1 1 d . . . . .
N217 N 0.6245(3) 0.0429(2) 0.28007(18) 0.0340(4) Uani 1 1 d . . . . .
H21A H 0.518(4) 0.013(3) 0.252(3) 0.054(8) Uiso 1 1 d . . . . .
H21B H 0.739(5) -0.034(4) 0.292(3) 0.054(8) Uiso 1 1 d . . . . .
C111 C 0.8138(3) 0.48454(19) 0.84687(17) 0.0217(4) Uani 1 1 d . . . . .
C112 C 0.7301(3) 0.60178(19) 0.92448(17) 0.0207(3) Uani 1 1 d . . . . .
H112 H 0.6091 0.6004 0.9793 0.025 Uiso 1 1 calc R . . . .
C113 C 0.8269(3) 0.72163(19) 0.92062(17) 0.0213(4) Uani 1 1 d . . . . .
C114 C 1.0038(3) 0.7263(2) 0.84211(19) 0.0259(4) Uani 1 1 d . . . . .
H114 H 1.0683 0.8091 0.8410 0.031 Uiso 1 1 calc R . . . .
C115 C 1.0844(3) 0.6067(2) 0.7650(2) 0.0287(4) Uani 1 1 d . . . . .
H115 H 1.2055 0.6081 0.7102 0.034 Uiso 1 1 calc R . . . .
C116 C 0.9909(3) 0.4847(2) 0.76678(19) 0.0264(4) Uani 1 1 d . . . . .
H116 H 1.0473 0.4031 0.7141 0.032 Uiso 1 1 calc R . . . .
C211 C 0.6714(3) 0.2299(2) 0.56872(18) 0.0266(4) Uani 1 1 d . . . . .
C212 C 0.7178(3) 0.1339(2) 0.46929(18) 0.0257(4) Uani 1 1 d . . . . .
H212 H 0.8437 0.0685 0.4583 0.031 Uiso 1 1 calc R . . . .
C213 C 0.5784(3) 0.1333(2) 0.38453(18) 0.0267(4) Uani 1 1 d . . . . .
C214 C 0.3956(3) 0.2306(3) 0.40369(19) 0.0336(5) Uani 1 1 d . . . . .
H214 H 0.2984 0.2308 0.3480 0.040 Uiso 1 1 calc R . . . .
C215 C 0.3548(3) 0.3266(3) 0.5029(2) 0.0425(6) Uani 1 1 d . . . . .
H215 H 0.2297 0.3931 0.5138 0.051 Uiso 1 1 calc R . . . .
C216 C 0.4921(3) 0.3283(3) 0.5873(2) 0.0387(5) Uani 1 1 d . . . . .
H216 H 0.4634 0.3950 0.6554 0.046 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'
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'
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
O12 P1 O11 105.43(8) . . ?
O13 P1 O11 104.10(7) . . ?
O13 P1 O12 111.25(8) . . ?
O14 P1 O11 111.22(8) . . ?
O14 P1 O12 105.24(8) . . ?
O14 P1 O13 118.93(8) . . ?
C111 O11 P1 125.98(12) . . ?
C211 O12 P1 124.13(12) . . ?
H11A N117 H11B 111(2) . . ?
H11A N117 H11C 109(2) . . ?
H11B N117 H11C 103(2) . . ?
C113 N117 H11A 108.8(15) . . ?
C113 N117 H11B 113.2(16) . . ?
C113 N117 H11C 111.9(16) . . ?
H21A N217 H21B 117(3) . . ?
C213 N217 H21A 115.8(18) . . ?
C213 N217 H21B 110.4(17) . . ?
C112 C111 O11 115.74(16) . . ?
C112 C111 C116 121.39(16) . . ?
C116 C111 O11 122.85(16) . . ?
C111 C112 H112 120.8 . . ?
C111 C112 C113 118.45(16) . . ?
C113 C112 H112 120.8 . . ?
C112 C113 N117 119.61(16) . . ?
C114 C113 N117 118.38(16) . . ?
C114 C113 C112 122.00(17) . . ?
C113 C114 H114 120.9 . . ?
C113 C114 C115 118.24(16) . . ?
C115 C114 H114 120.9 . . ?
C114 C115 H115 119.4 . . ?
C114 C115 C116 121.11(18) . . ?
C116 C115 H115 119.4 . . ?
C111 C116 C115 118.80(18) . . ?
C111 C116 H116 120.6 . . ?
C115 C116 H116 120.6 . . ?
C212 C211 O12 116.31(17) . . ?
C216 C211 O12 121.34(18) . . ?
C216 C211 C212 122.30(18) . . ?
C211 C212 H212 120.2 . . ?
C211 C212 C213 119.65(18) . . ?
C213 C212 H212 120.2 . . ?
N217 C213 C212 120.80(19) . . ?
N217 C213 C214 120.63(18) . . ?
C214 C213 C212 118.50(18) . . ?
C213 C214 H214 119.8 . . ?
C215 C214 C213 120.43(19) . . ?
C215 C214 H214 119.8 . . ?
C214 C215 H215 119.2 . . ?
C214 C215 C216 121.5(2) . . ?
C216 C215 H215 119.2 . . ?
C211 C216 C215 117.6(2) . . ?
C211 C216 H216 121.2 . . ?
C215 C216 H216 121.2 . . ?
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
P1 O11 1.6088(14) . ?
P1 O12 1.5935(14) . ?
P1 O13 1.4903(13) . ?
P1 O14 1.4751(14) . ?
O11 C111 1.392(2) . ?
O12 C211 1.404(2) . ?
N117 H11A 0.90(2) . ?
N117 H11B 0.89(3) . ?
N117 H11C 0.92(3) . ?
N117 C113 1.454(2) . ?
N217 H21A 0.93(3) . ?
N217 H21B 0.95(3) . ?
N217 C213 1.387(3) . ?
C111 C112 1.380(3) . ?
C111 C116 1.387(3) . ?
C112 H112 0.9500 . ?
C112 C113 1.386(2) . ?
C113 C114 1.384(3) . ?
C114 H114 0.9500 . ?
C114 C115 1.389(3) . ?
C115 H115 0.9500 . ?
C115 C116 1.391(3) . ?
C116 H116 0.9500 . ?
C211 C212 1.378(3) . ?
C211 C216 1.377(3) . ?
C212 H212 0.9500 . ?
C212 C213 1.400(3) . ?
C213 C214 1.391(3) . ?
C214 H214 0.9500 . ?
C214 C215 1.377(3) . ?
C215 H215 0.9500 . ?
C215 C216 1.388(3) . ?
C216 H216 0.9500 . ?
