Dihydrogen phosphate-containing dinuclear double assemblies that demonstrate phosphate reactivity to the tetrafluoroborate anion.
Faulkner, Robert A.; Patmore, Nathan J.; Rice, Craig R.; Slater, Christopher; Chemical communications (Cambridge, England) 54 (2018) 9159–9162; doi:10.1039/c8cc04900a

data_7122002
_publ_section_title
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 Dihydrogen phosphate-containing dinuclear double assemblies that
 demonstrate phosphate reactivity to the tetrafluoroborate anion.
;
_journal_issue                   66
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              9159
_journal_page_last               9162
_journal_paper_doi               10.1039/c8cc04900a
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'C40 H42 Cu2 N12 O4 P S4, 3(C F3 O3 S)'
_chemical_formula_sum            'C43 H42 Cu2 F9 N12 O13 P S7'
_chemical_formula_weight         1488.40
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_date             2016-06-08
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2018-06-16 deposited with the CCDC.
2018-07-18 downloaded from the CCDC.
;
_cell_angle_alpha                93.102(18)
_cell_angle_beta                 103.018(14)
_cell_angle_gamma                95.287(15)
_cell_formula_units_Z            2
_cell_length_a                   14.629(5)
_cell_length_b                   15.453(6)
_cell_length_c                   17.397(6)
_cell_measurement_reflns_used    9275
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      33.11
_cell_measurement_theta_min      2.16
_cell_volume                     3804(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.9995
_diffrn_measured_fraction_theta_max 0.9939
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0777
_diffrn_reflns_av_unetI/netI     0.0925
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            114289
_diffrn_reflns_theta_full        26.0000
_diffrn_reflns_theta_max         30.44
_diffrn_reflns_theta_min         1.85
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.848
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.2994
_exptl_crystal_description       block
_exptl_crystal_F_000             1512.1201
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.6065
_refine_diff_density_min         -2.0660
_refine_diff_density_rms         0.2181
_refine_ls_d_res_high            0.7014
_refine_ls_d_res_low             11.0148
_refine_ls_goodness_of_fit_ref   1.1000
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    77
_refine_ls_number_parameters     858
_refine_ls_number_reflns         22936
_refine_ls_number_restraints     87
_refine_ls_restrained_S_all      1.0978
_refine_ls_R_factor_all          0.1334
_refine_ls_R_factor_gt           0.0762
_refine_ls_shift/su_max          0.0007
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1145P)^2^+2.7898P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1957
_refine_ls_wR_factor_ref         0.2317
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              20
_reflns_limit_h_min              -20
_reflns_limit_k_max              21
_reflns_limit_k_min              -21
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                13386
_reflns_number_total             22936
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c8cc04900a2.cif
_cod_data_source_block           mo_Chris_Lbeda_CuPO4_0m_a
_cod_depositor_comments
'Adding full bibliography for 7122000--7122004.cif.'
_cod_database_code               7122002
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H) groups
2. Rigid bond restraints
 O8, O1A, O2A, O3A, O1B, O2B, O3B
 with sigma for 1-2 distances of 0.003 and sigma for 1-3 distances of 0.006
 O8, F1A, F2A, F3A, F1B, F2B, F3B, C1A, C1B
 with sigma for 1-2 distances of 0.003 and sigma for 1-3 distances of 0.006
 C6, C4, C3, C2
 with sigma for 1-2 distances of 0.003 and sigma for 1-3 distances of 0.006
3. Uiso/Uaniso restraints and constraints
O8 \\sim O1A \\sim O2A \\sim O3A \\sim O1B \\sim O2B \\sim O3B: within 2A with
sigma of 0.003 and sigma for terminal atoms of 0.006
O8 \\sim F1A \\sim F2A \\sim F3A \\sim F1B \\sim F2B \\sim F3B \\sim C1A \\sim
C1B: within 2A with sigma of 0.003 and sigma for terminal atoms of 0.006
Uanis(O3B) \\sim Ueq, Uanis(O2B) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C18) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1
Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C4) \\sim Ueq: with sigma of
0.05 and sigma for terminal atoms of 0.1
4. Others
 Sof(S1B)=Sof(O1B)=Sof(O2B)=Sof(C1B)=Sof(F1B)=Sof(O3B)=Sof(F2B)=Sof(F3B)=1-
 FVAR(1)
 Sof(C1A)=Sof(F1A)=Sof(F2A)=Sof(F3A)=Sof(O1A)=Sof(O2A)=Sof(O3A)=Sof(S1A)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C9(H9a,H9b), C10(H10a,H10b), C11(H11a,H11b), C12(H12a,H12b), C29(H29a,H29b),
 C30(H30a,H30b), C31(H31a,H31b), C32(H32a,H32b)
5.b Aromatic/amide H refined with riding coordinates:
 N3(H3), N4(H4), N9(H9), N10(H10), C1(H1a), C2(H2), C3(H3a), C4(H4b), C7(H7),
 C14(H14), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23),
  C24(H24), C27(H27), C34(H34), C37(H37), C38(H38), C39(H39), C40(H40)
5.c Idealised tetrahedral OH refined as rotating group:
 O1(H1), O4(H4a)
;
_olex2_submission_special_instructions 'No special instructions were received'