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_7122004
_publ_section_title
;
 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
'2(C54 H48 B Cu3 F3 N18 O4 P S6), 3(B F4), 6(C H3 N O2)'
_chemical_formula_sum            'C114 H114 B5 Cu6 F18 N42 O20 P2 S12'
_chemical_formula_weight         3616.55
_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             2016-02-26
_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                78.661(7)
_cell_angle_beta                 85.813(9)
_cell_angle_gamma                78.326(7)
_cell_formula_units_Z            2
_cell_length_a                   12.3871(8)
_cell_length_b                   24.199(2)
_cell_length_c                   32.271(4)
_cell_measurement_reflns_used    9809
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      68.32
_cell_measurement_theta_min      2.80
_cell_volume                     9282.8(15)
_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 0.9774
_diffrn_measured_fraction_theta_max 0.9774
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1127
_diffrn_reflns_av_unetI/netI     0.0914
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            132190
_diffrn_reflns_theta_full        68.7210
_diffrn_reflns_theta_max         68.72
_diffrn_reflns_theta_min         2.56
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.867
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.2937
_exptl_crystal_description       block
_exptl_crystal_F_000             3666.8836
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.8506
_refine_diff_density_min         -1.6788
_refine_diff_density_rms         0.2042
_refine_ls_d_res_high            0.8273
_refine_ls_d_res_low             17.2769
_refine_ls_goodness_of_fit_ref   1.2535
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    208
_refine_ls_number_parameters     2014
_refine_ls_number_reflns         33538
_refine_ls_number_restraints     121
_refine_ls_restrained_S_all      1.2511
_refine_ls_R_factor_all          0.1337
_refine_ls_R_factor_gt           0.0997
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2929
_refine_ls_wR_factor_ref         0.3299
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              29
_reflns_limit_k_min              -28
_reflns_limit_l_max              38
_reflns_limit_l_min              0
_reflns_number_gt                23849
_reflns_number_total             33538
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c8cc04900a2.cif
_cod_data_source_block           cu_Chris_BF4PO4_4_0m_a
_cod_depositor_comments
'Adding full bibliography for 7122000--7122004.cif.'
_cod_original_cell_volume        9283.1(15)
_cod_database_code               7122004
_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 C(H,H,H) groups
2. Rigid bond restraints
 F8, F22, F19, B6, F20, F21
 with sigma for 1-2 distances of 0.003 and sigma for 1-3 distances of 0.006
 C42
 with sigma for 1-2 distances of 0.003 and sigma for 1-3 distances of 0.006
 C11, C15, C16, C17
 with sigma for 1-2 distances of 0.003 and sigma for 1-3 distances of 0.006
3. Uiso/Uaniso restraints and constraints
F8 \\sim F22 \\sim F19 \\sim B6 \\sim F20 \\sim F21: within 2A with sigma of
0.003 and sigma for terminal atoms of 0.006
C42: within 2A with sigma of 0.003 and sigma for terminal atoms of 0.006
C11 \\sim C15 \\sim C16 \\sim C17: within 2A with sigma of 0.003 and sigma for
terminal atoms of 0.006
Uanis(N44) \\sim Ueq, Uanis(O23) \\sim Ueq, Uanis(O24) \\sim Ueq, Uanis(C117)
\\sim Ueq, : with sigma of 0.05 and sigma for terminal atoms of 0.1
Uanis(N48) \\sim Ueq, Uanis(O11) \\sim Ueq, Uanis(O12) \\sim Ueq, Uanis(C109)
\\sim Ueq, : with sigma of 0.05 and sigma for terminal atoms of 0.1
Uanis(N47) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C111) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C108) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C117) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: N44(0.5) N47(0.5) O23(0.5) O24(0.5) O31(0.5) O32(0.5) C111(0.5)
 H11j(0.5) H11k(0.5) H11l(0.5) C117(0.5) H11g(0.5) H11h(0.5) H11i(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C9(H9a,H9b), C10(H10a,H10b), C27(H27a,H27b), C0aa(H0aa,H0ab), C45(H45a,H45b),
 C46(H46a,H46b), C63(H63a,H63b), C64(H64a,H64b), C80(H80a,H80b), C81(H81a,H81b),
  C98(H98a,H98b), C99(H99a,H99b)
5.b Aromatic/amide H refined with riding coordinates:
 N3(H3), N4(H4), N9(H9), N10(H10), N15(H15), N16(H16), N21(H21a), N22(H22a),
 N27(H27), N28(H28), N33(H33a), N34(H34a), C1(H1), C2(H2), C3(H3a), C4(H4a),
 C7(H7), C12(H12), C15(H15a), C16(H16a), C17(H17), C18(H18), C19(H19), C20(H20),
  C21(H21), C22(H22), C25(H25), C30(H30), C33(H33), C34(H34), C35(H35),
 C36(H36), C37(H37), C38(H38), C39(H39), C40(H40), C43(H43), C047(H047),
 C48(H48), C51(H51), C52(H52), C53(H53), C54(H54), C55(H55), C56(H56), C57(H57),
  C58(H58), C61(H61), C68(H68), C69(H69), C70(H70), C71(H71), C72(H72),
 C73(H73), C74(H74), C75(H75), C78(H78), C83(H83), C86(H86), C87(H87), C88(H88),
  C89(H89), C90(H90), C91(H91), C92(H92), C93(H93), C96(H96), C101(H101),
 C104(H104), C105(H105), C106(H106), C107(H107)
5.c Idealised Me refined as rotating group:
 C108(H10c,H10d,H10e), C109(H10f,H10g,H10h), C110(H11d,H11e,H11f), C111(H11j,
 H11k,H11l), C113(H11a,H11b,H11c), C117(H11g,H11h,H11i), C05N(H05a,H05b,H05c)
;
_olex2_submission_special_instructions 'No special instructions were received'