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_7122001
_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
'C36 H34 Cu2 N12 O4 P S4, 3(C F3 O3 S), C N O2, 0.86(N1), 0.74(O)'
_chemical_formula_sum            'C40 H34 Cu2 F9 N13.858 O15.743 P S7'
_chemical_formula_weight         1514.22
_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             2016-03-15
_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                99.030(16)
_cell_angle_beta                 108.218(16)
_cell_angle_gamma                92.693(12)
_cell_formula_units_Z            2
_cell_length_a                   11.358(4)
_cell_length_b                   16.280(5)
_cell_length_c                   16.681(7)
_cell_measurement_reflns_used    9113
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.50
_cell_measurement_theta_min      2.28
_cell_volume                     2878.3(18)
_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 0.9916
_diffrn_measured_fraction_theta_max 0.9906
_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  0.0829
_diffrn_reflns_av_unetI/netI     0.0883
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            80975
_diffrn_reflns_theta_full        30.6865
_diffrn_reflns_theta_max         30.69
_diffrn_reflns_theta_min         1.92
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.127
_exptl_absorpt_correction_T_max  0.88
_exptl_absorpt_correction_T_min  0.77
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.7470
_exptl_crystal_description       block
_exptl_crystal_F_000             1530.0797
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.6254
_refine_diff_density_min         -2.0257
_refine_diff_density_rms         0.2795
_refine_ls_d_res_high            0.6963
_refine_ls_d_res_low             10.5876
_refine_ls_goodness_of_fit_ref   1.0732
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    66
_refine_ls_number_parameters     886
_refine_ls_number_reflns         17674
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.0717
_refine_ls_R_factor_all          0.1299
_refine_ls_R_factor_gt           0.0744
_refine_ls_shift/su_max          0.0027
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0812P)^2^+6.0513P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1587
_refine_ls_wR_factor_ref         0.1923
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              15
_reflns_limit_h_min              -16
_reflns_limit_k_max              22
_reflns_limit_k_min              -23
_reflns_limit_l_max              23
_reflns_limit_l_min              0
_reflns_number_gt                11284
_reflns_number_total             17674
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c8cc04900a2.cif
_cod_data_source_block           mo_Chris_LedaPO4trif_2_0m_a
_cod_depositor_comments
'Adding full bibliography for 7122000--7122004.cif.'
_cod_original_cell_volume        2878.4(18)
_cod_database_code               7122001
_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
 C25, O16, N14, O17
 with sigma for 1-2 distances of 0.003 and sigma for 1-3 distances of 0.006
 H36, O3, O1A, O2A
 with sigma for 1-2 distances of 0.003 and sigma for 1-3 distances of 0.006
3. Uiso/Uaniso restraints and constraints
C25 \\sim O16 \\sim N14 \\sim O17: within 2A with sigma of 0.003 and sigma for
terminal atoms of 0.006
O3 \\sim O2A \\sim O1A: within 2A with sigma of 0.003 and sigma for terminal
atoms of 0.006
Uanis(C40) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O16) \\sim Ueq, Uanis(N14) \\sim Ueq, Uanis(O17) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C1B) \\sim Ueq, Uanis(O1A) \\sim Ueq, Uanis(C1A) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(O3A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(C1B)=Sof(S1B)=Sof(O1B)=Sof(O2B)=Sof(O3B)=Sof(F1B)=Sof(F2B)=Sof(F3B)=
 Sof(N14)=1-FVAR(1)
 Sof(C1A)=Sof(F1A)=Sof(F2A)=Sof(F3A)=Sof(O1A)=Sof(O2A)=Sof(S1A)=Sof(O3A)=FVAR(1)
 Sof(O16)=Sof(O17)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C9(H9a,H9b), C10(H10a,H10b), C27(H27a,H27b), C28(H28a,H28b)
5.b Aromatic/amide H refined with riding coordinates:
 N3(H3), N4(H4), N9(H9), N10(H10), C1(H1), C2(H2), C3(H3b), C4(H4b), C7(H7),
 C12(H12), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21),
  C22(H22), C25(H25), C30(H30), C33(H33), C34(H34), C35(H35), C36(H36)
5.c Idealised tetrahedral OH refined as rotating group:
 O3(H3a), O4(H4a)
;
_olex2_submission_special_instructions 'No special instructions were received'