Assembly of BF4−, PF6−, ClO4− and F− with trinuclear copper(i) acetylide complexes bearing amide groups: structural diversity, photophysics and anion binding properties
Shi, Hua-Yun; Huang, Yong-Liang; Sun, Jia-Kai; Jiang, Ji-Jun; Luo, Zhi-Xing; Ling, Hui-Tao; Lam, Chi-Keung; Chao, Hsiu-Yi; RSC Advances 5 (2015) 89669–; doi:10.1039/C5RA18534C

data_7235997
_publ_section_title
;
 Assembly of BF4&#x2212;, PF6&#x2212;, ClO4&#x2212; and F&#x2212; with
 trinuclear copper(i) acetylide complexes bearing amide groups: structural
 diversity, photophysics and anion binding properties
;
_journal_issue                   109
_journal_name_full               'RSC Advances'
_journal_page_first              89669
_journal_paper_doi               10.1039/C5RA18534C
_journal_volume                  5
_journal_year                    2015
_chemical_formula_moiety         'C105 H83.43 Cu3 N4 O6 P6, B1 F4'
_chemical_formula_sum            'C105 H83.5 B Cu3 F4 N4 O6 P6'
_chemical_formula_weight         1960.51
_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_Hall           '-P 2ab 2ac'
_space_group_name_H-M_alt        'P c c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-07-28
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4813)
;
_audit_update_record
;
2015-09-01 deposited with the CCDC.
2015-10-14 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   22.4406(2)
_cell_length_b                   37.5572(3)
_cell_length_c                   23.51115(19)
_cell_measurement_temperature    293(2)
_cell_volume                     19815.3(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL-1997 (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS-1997 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0365
_diffrn_reflns_av_unetI/netI     0.0245
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            76185
_diffrn_reflns_theta_full        63.00
_diffrn_reflns_theta_max         63.00
_diffrn_reflns_theta_min         2.97
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.169
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             8060
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_platon_squeeze_details
;
;
_refine_diff_density_max         1.613
_refine_diff_density_min         -1.040
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1239
_refine_ls_number_reflns         16018
_refine_ls_number_restraints     2844
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0771
_refine_ls_R_factor_gt           0.0733
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0795P)^2^+105.3148P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1948
_refine_ls_wR_factor_ref         0.1972
_reflns_number_gt                14663
_reflns_number_total             16018
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ra18534c2.cif
_cod_data_source_block           squeezed
_cod_original_formula_sum        'C105 H83.50 B Cu3 F4 N4 O6 P6'
_cod_database_code               7235997
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H2(0.072) H3(0.077) H4(0.073) H6(0.071) H2A(0.068) H3A(0.07)
 H4A(0.076) H5A(0.082) H6A(0.077) H12A(0.039) H12B(0.041) H10A(0.035)
 H41A(0.047) H41B(0.047) H72A(0.05) H71A(0.053) H45A(0.057) H18A(0.069)
 H10B(0.04) H77A(0.066) H10C(0.037) H11A(0.053) H23A(0.052) H10D(0.039)
 H63A(0.045) H30A(0.049) H87A(0.042) H10E(0.039) H51A(0.06) H44A(0.062)
 H11B(0.051) H52A(0.051) H1A(0.054) H70A(0.048) H90A(0.048) H65A(0.06)
 H13A(0.076) H19A(0.079) H69A(0.041) H64A(0.057) H57A(0.04) H76A(0.053)
 H11C(0.051) H82A(0.038) H82B(0.038) H86A(0.041) H80A(0.044) H43A(0.065)
 H67A(0.045) H36A(0.088) H95A(0.046) H81A(0.033) H81B(0.033) H58A(0.053)
 H27A(0.051) H33A(0.044) H66A(0.054) H17A(0.055) H97A(0.05) H32A(0.051)
 H29A(0.042) H73A(0.044) H61A(0.044) H15A(0.066) H37A(0.099) H47A(0.071)
 H12C(0.065) H33B(0.044) H21A(0.06) H31A(0.05) H60A(0.053) H98A(0.048)
 H20A(0.073) H89A(0.045) H24A(0.064) H59A(0.055) H14A(0.081) H48A(0.086)
 H93A(0.049) H78A(0.067) H50A(0.08) H79A(0.06) H42A(0.062) H26A(0.062)
 H35A(0.073) H25A(0.064) H38A(0.108) H39A(0.088)
 Fixed X: H2(0.7198) H3(0.802) H4(0.8245) H6(0.6824) H2A(0.6681) H3A(0.7541)
 H4A(0.8349) H5A(0.8299) H6A(0.7439) H12A(0.5977) H12B(0.5138) H10A(0.4687)
 H41A(0.6717) H41B(0.6363) H72A(0.144) H71A(0.1463) H45A(0.5863) H18A(0.5633)
 H10B(0.4116) H77A(0.378) H10C(0.4556) H11A(0.588) H23A(0.4537) H10D(0.5004)
 H63A(0.4024) H30A(0.3714) H87A(0.6605) H10E(0.4863) H51A(0.606) H44A(0.5858)
 H11B(0.5265) H52A(0.5828) H1A(0.4889) H70A(0.2278) H90A(0.481) H65A(0.243)
 H13A(0.6329) H19A(0.5717) H69A(0.3052) H64A(0.3356) H57A(0.3931) H76A(0.3904)
 H11C(0.5697) H82A(0.4654) H82B(0.4775) H86A(0.6197) H80A(0.2573) H43A(0.536)
 H67A(0.282) H36A(0.6475) H95A(0.7094) H81A(0.3299) H81B(0.3) H58A(0.365)
 H27A(0.3125) H33A(0.427) H66A(0.2156) H17A(0.5623) H97A(0.6398) H32A(0.461)
 H29A(0.3602) H73A(0.2229) H61A(0.3632) H15A(0.665) H37A(0.7106) H47A(0.721)
 H12C(0.5516) H33B(0.4493) H21A(0.5856) H31A(0.4215) H60A(0.3315) H98A(0.6279)
 H20A(0.5775) H89A(0.5218) H24A(0.4316) H59A(0.3308) H14A(0.6896) H48A(0.7418)
 H93A(0.7153) H78A(0.3073) H50A(0.6834) H79A(0.2454) H42A(0.4858) H26A(0.2916)
 H35A(0.5771) H25A(0.3518) H38A(0.6861) H39A(0.6198)
 Fixed Y: H2(0.5786) H3(0.5773) H4(0.6264) H6(0.678) H2A(0.5846) H3A(0.5742)
 H4A(0.6123) H5A(0.6608) H6A(0.6712) H12A(0.3998) H12B(0.8411) H10A(0.7698)
 H41A(0.5939) H41B(0.5715) H72A(0.6055) H71A(0.6671) H45A(0.7131) H18A(0.4973)
 H10B(0.8949) H77A(0.4796) H10C(0.7125) H11A(0.943) H23A(0.5247) H10D(0.8019)
 H63A(0.5704) H30A(0.6922) H87A(0.4775) H10E(0.7448) H51A(0.7488) H44A(0.7746)
 H11B(0.6537) H52A(0.7011) H1A(0.7056) H70A(0.6982) H90A(0.4921) H65A(0.5551)
 H13A(0.6762) H19A(0.4512) H69A(0.6678) H64A(0.5344) H57A(0.7028) H76A(0.5404)
 H11C(0.882) H82A(0.651) H82B(0.6128) H86A(0.5336) H80A(0.5461) H43A(0.8009)
 H67A(0.6495) H36A(0.5619) H95A(0.3627) H81A(0.6338) H81B(0.5967) H58A(0.7615)
 H27A(0.557) H33A(0.9562) H66A(0.6126) H17A(0.5555) H97A(0.2892) H32A(0.6102)
 H29A(0.6615) H73A(0.5748) H61A(0.684) H15A(0.5904) H37A(0.5983) H47A(0.6474)
 H12C(0.6906) H33B(0.5791) H21A(0.5217) H31A(0.6668) H60A(0.7418) H98A(0.3505)
 H20A(0.4635) H89A(0.4365) H24A(0.4662) H59A(0.7806) H14A(0.6266) H48A(0.6951)
 H93A(0.3013) H78A(0.4514) H50A(0.745) H79A(0.4849) H42A(0.7674) H26A(0.4985)
 H35A(0.5859) H25A(0.4535) H38A(0.6574) H39A(0.6832)
 Fixed Z: H2(0.2733) H3(0.3331) H4(0.3891) H6(0.3257) H2A(0.3242) H3A(0.3765)
 H4A(0.3678) H5A(0.3068) H6A(0.2545) H12A(0.3008) H12B(0.1539) H10A(0.0699)
 H41A(0.1754) H41B(0.2207) H72A(0.3366) H71A(0.3424) H45A(0.32) H18A(0.0074)
 H10B(0.0368) H77A(0.3135) H10C(0.102) H11A(0.1051) H23A(0.1603) H10D(0.2303)
 H63A(0.413) H30A(0.0083) H87A(0.3589) H10E(0.2622) H51A(0.1639) H44A(0.3294)
 H11B(0.0997) H52A(0.2213) H1A(0.4618) H70A(0.3083) H90A(0.2633) H65A(0.485)
 H13A(-0.0327) H19A(0.0707) H69A(0.2646) H64A(0.4609) H57A(0.3011) H76A(0.3085)
 H11C(0.114) H82A(0.4499) H82B(0.4255) H86A(0.3483) H80A(0.1949) H43A(0.4021)
 H67A(0.415) H36A(0.4703) H95A(0.4318) H81A(0.1667) H81B(0.1548) H58A(0.314)
 H27A(0.0682) H33A(0.0329) H66A(0.4619) H17A(0.0383) H97A(0.2881) H32A(-0.0582)
 H29A(0.0928) H73A(0.2961) H61A(0.4669) H15A(0.0629) H37A(0.5179) H47A(0.1567)
 H12C(0.0245) H33B(0.0259) H21A(0.1972) H31A(-0.0668) H60A(0.4787) H98A(0.2813)
 H20A(0.1671) H89A(0.2732) H24A(0.1364) H59A(0.4016) H14A(-0.0123) H48A(0.0981)
 H93A(0.4413) H78A(0.2576) H50A(0.0996) H79A(0.2008) H42A(0.467) H26A(0.0458)
 H35A(0.41) H25A(0.0804) H38A(0.5278) H39A(0.4633)
;