#------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/05/2010534.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2010534
loop_
_publ_author_name
'Hubin, Timothy J.'
'Alcock, Nathaniel W.'
'Busch, Daryle H.'
_publ_section_title
;
 Copper(I) and copper(II) complexes of an ethylene cross-bridged cyclam
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              37
_journal_page_last               39
_journal_paper_doi               10.1107/S010827019901255X
_journal_volume                  56
_journal_year                    2000
_chemical_formula_iupac          '[Cu (C2 H3 N) (C26 H38 N4)] 2P F6'
_chemical_formula_sum            'C28 H41 Cu F12 N5 P2'
_chemical_formula_weight         801.14
_chemical_name_systematic
;
[acetonitrile(4,11-dibenzyl-1,4,8,11-
tetraazabicyclo[6.6.2]hexadecane-κ⁴N)]copper(II)
bis(hexafluorophosphate)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                101.2360(10)
_cell_angle_beta                 101.1050(10)
_cell_angle_gamma                109.1570(10)
_cell_formula_units_Z            2
_cell_length_a                   9.9695(4)
_cell_length_b                   10.5610(5)
_cell_length_c                   17.7607(8)
_cell_measurement_reflns_used    7334
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      3
_cell_volume                     1664.83(13)
_computing_cell_refinement       'SAINT (Siemens, 1995)'
_computing_data_collection       'SMART (Siemens, 1994)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 1997b)'
_diffrn_ambient_temperature      180(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full .874
_diffrn_measured_fraction_theta_max .874
_diffrn_measurement_device_type  'Siemens SMART'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .015
_diffrn_reflns_av_sigmaI/netI    .022
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            10176
_diffrn_reflns_theta_full        28.53
_diffrn_reflns_theta_max         28.53
_diffrn_reflns_theta_min         1.22
_diffrn_standards_decay_%        nil
_exptl_absorpt_coefficient_mu    .849
_exptl_absorpt_correction_T_max  .881
_exptl_absorpt_correction_T_min  .774
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.598
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             822
_exptl_crystal_size_max          .4
_exptl_crystal_size_mid          .2
_exptl_crystal_size_min          .2
_refine_diff_density_max         1.087
_refine_diff_density_min         -.882
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     434
_refine_ls_number_reflns         7384
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          .064
_refine_ls_R_factor_gt           .055
_refine_ls_shift/su_max          .006
_refine_ls_shift/su_mean         .001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.0648P)²+3.3905P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .146
_reflns_number_gt                6457
_reflns_number_total             7384
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ha1270.cif
_cod_data_source_block           II
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_geom_bond_publ_flag' value 'Y' changed to 'y' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (5 times).

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_geom_bond_publ_flag' value 'Y' changed to 'y'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (5
times).

'_geom_angle_publ_flag' value 'Y' changed to 'y' according
to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29 (10 times).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C28 H41 Cu F12 N5  P2'
_cod_database_code               2010534
_cod_database_fobs_code          2010534
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
Cu1 .72383(4) .64532(4) .74953(2) .02522(11) Uani d . 1 . . Cu
N1 .6664(3) .7778(2) .83199(14) .0254(5) Uani d . 1 . . N
N4 .9319(3) .7114(3) .83699(15) .0297(5) Uani d . 1 . . N
N8 .7695(3) .5127(3) .66624(15) .0307(5) Uani d . 1 . . N
N11 .6508(3) .4772(3) .79689(15) .0292(5) Uani d . 1 . . N
N31 .7844(3) .7929(3) .68970(15) .0337(6) Uani d . 1 . . N
C2 .7868(3) .8212(3) .90787(17) .0298(6) Uani d . 1 . . C
H2A .7629 .7494 .9370 .036 Uiso calc R 1 . . H
H2B .7932 .9100 .9423 .036 Uiso calc R 1 . . H
C3 .9367(3) .8403(3) .89103(19) .0328(6) Uani d . 1 . . C
H3A .9648 .9179 .8663 .039 Uiso calc R 1 . . H
H3B 1.0131 .8656 .9421 .039 Uiso calc R 1 . . H
C5 1.0591(3) .7446(4) .8024(2) .0372(7) Uani d . 1 . . C
H5A 1.1508 .7707 .8454 .045 Uiso calc R 1 . . H
H5B 1.0662 .8269 .7822 .045 Uiso calc R 1 . . H
C6 1.0512(4) .6258(4) .7343(2) .0414(8) Uani d . 1 . . C
H6A 1.0460 .5447 .7553 .050 Uiso calc R 1 . . H
H6B 1.1448 .6559 .7192 .050 Uiso calc R 1 . . H
C7 .9233(4) .5763(4) .6582(2) .0376(7) Uani d . 1 . . C
H7A .9291 .6571 .6366 .045 Uiso calc R 1 . . H
H7B .9384 .5068 .6181 .045 Uiso calc R 1 . . H
C9 .7521(4) .3819(3) .6913(2) .0363(7) Uani d . 1 . . C
H9A .8473 .3926 .7266 .044 Uiso calc R 1 . . H
H9B .7251 .3028 .6435 .044 Uiso calc R 1 . . H
C10 .6337(4) .3503(3) .73505(19) .0363(7) Uani d . 1 . . C
H10A .5351 .3145 .6961 .044 Uiso calc R 1 . . H
H10B .6396 .2767 .7610 .044 Uiso calc R 1 . . H
C12 .5035(4) .4523(3) .8130(2) .0344(7) Uani d . 1 . . C
H12A .4777 .3708 .8348 .041 Uiso calc R 1 . . H
H12B .4283 .4278 .7616 .041 Uiso calc R 1 . . H
C13 .4946(4) .5740(3) .8702(2) .0348(7) Uani d . 1 . . C
H13A .5697 .5981 .9216 .042 Uiso calc R 1 . . H
H13B .3964 .5433 .8804 .042 Uiso calc R 1 . . H
C14 .5177(3) .7054(3) .84260(19) .0310(6) Uani d . 1 . . C
H14A .4428 .6807 .7910 .037 Uiso calc R 1 . . H
H14B .4980 .7728 .8818 .037 Uiso calc R 1 . . H
C15 .9249(4) .5980(3) .87599(19) .0338(7) Uani d . 1 . . C
H15A .9829 .6404 .9327 .041 Uiso calc R 1 . . H
H15B .9723 .5395 .8502 .041 Uiso calc R 1 . . H
C16 .7673(4) .5035(3) .87228(18) .0332(6) Uani d . 1 . . C
H16A .7684 .4126 .8783 .040 Uiso calc R 1 . . H
H16B .7392 .5466 .9183 .040 Uiso calc R 1 . . H
C17 .6631(3) .9067(3) .80587(18) .0297(6) Uani d . 1 . . C
H17A .7649 .9633 .8067 .036 Uiso calc R 1 . . H
H17B .6017 .8750 .7498 .036 Uiso calc R 1 . . H
C18 .6056(3) 1.0007(3) .85457(18) .0307(6) Uani d . 1 . . C
C19 .6980(4) 1.1081(3) .9225(2) .0365(7) Uani d . 1 . . C
H19A .7990 1.1209 .9401 .044 Uiso calc R 1 . . H
C20 .6445(5) 1.1971(4) .9650(2) .0463(8) Uani d . 1 . . C
H20A .7085 1.2693 1.0115 .056 Uiso calc R 1 . . H
C21 .4983(5) 1.1801(4) .9392(2) .0480(9) Uani d . 1 . . C
H21A .4611 1.2397 .9683 .058 Uiso calc R 1 . . H
C22 .4066(4) 1.0765(4) .8712(3) .0487(9) Uani d . 1 . . C
H22A .3064 1.0660 .8531 .058 Uiso calc R 1 . . H
C23 .4590(4) .9872(4) .8287(2) .0413(8) Uani d . 1 . . C
H23A .3946 .9164 .7818 .050 Uiso calc R 1 . . H
C24 .6646(4) .4814(3) .58505(17) .0333(6) Uani d . 1 . . C
H24A .6931 .5655 .5657 .040 Uiso calc R 1 . . H
H24B .6763 .4060 .5473 .040 Uiso calc R 1 . . H
C25 .5041(4) .4379(3) .58379(18) .0332(6) Uani d . 1 . . C
C26 .4082(4) .2973(4) .5560(2) .0416(8) Uani d . 1 . . C
H26A .4442 .2279 .5370 .050 Uiso calc R 1 . . H
C27 .2610(5) .2586(4) .5560(2) .0495(9) Uani d . 1 . . C
H27A .1974 .1628 .5378 .059 Uiso calc R 1 . . H
C28 .2062(4) .3584(4) .5825(2) .0489(9) Uani d . 1 . . C
H28A .1056 .3312 .5829 .059 Uiso calc R 1 . . H
C29 .2987(4) .4981(4) .6083(2) .0402(7) Uani d . 1 . . C
H29A .2612 .5671 .6257 .048 Uiso calc R 1 . . H
C30 .4456(4) .5372(3) .60880(18) .0343(7) Uani d . 1 . . C
H30A .5079 .6334 .6265 .041 Uiso calc R 1 . . H
C32 .8336(5) .8881(4) .6642(2) .0450(8) Uani d . 1 . . C
C33 .8972(7) 1.0057(5) .6355(3) .0739(16) Uani d . 1 . . C
H33A .9590 .9848 .6020 .111 Uiso calc R 1 . . H
H33B .9578 1.0875 .6809 .111 Uiso calc R 1 . . H
H33C .8181 1.0252 .6038 .111 Uiso calc R 1 . . H
P1 .25685(13) .86859(11) .57564(6) .0501(3) Uani d . 1 . . P
P2 1.09189(9) .28008(9) .86784(5) .03456(19) Uani d . 1 . . P
F11 .1276(4) .9107(3) .53289(18) .0757(8) Uani d . 1 . . F
F12 .3798(4) .8247(3) .6198(3) .1284(19) Uani d . 1 . . F
F13 .1839(5) .8581(5) .6465(2) .1230(16) Uani d . 1 . . F
F14 .3239(6) .8803(7) .5041(3) .164(2) Uani d . 1 . . F
F15 .1558(5) .7101(3) .5317(3) .1265(18) Uani d . 1 . . F
F16 .3562(4) 1.0242(3) .6212(2) .0884(10) Uani d . 1 . . F
F21 1.1366(3) .3811(5) .8157(3) .1260(18) Uani d . 1 . . F
F22 1.0440(3) .1769(3) .92155(19) .0792(9) Uani d . 1 . . F
F23 1.2569(3) .3287(3) .92069(18) .0769(9) Uani d . 1 . . F
F24 .9256(3) .2306(3) .81601(16) .0666(7) Uani d . 1 . . F
F25 1.0655(5) .3923(4) .92798(19) .1120(15) Uani d . 1 . . F
F26 1.1094(6) .1584(5) .81033(19) .143(2) Uani d . 1 . . F
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F .0171 .0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P .1023 .0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu .3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O .0106 .0060 '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_publ_flag
N31 Cu1 N8 88.19(10) y
N31 Cu1 N11 173.04(10) y
N8 Cu1 N11 86.28(10) y
N31 Cu1 N1 91.98(10) y
N8 Cu1 N1 177.33(10) y
N11 Cu1 N1 93.35(9) y
N31 Cu1 N4 97.76(10) y
N8 Cu1 N4 95.25(10) y
N11 Cu1 N4 86.96(10) y
N1 Cu1 N4 87.37(10) y
C2 N1 C14 111.7(2) ?
C2 N1 C17 109.7(2) ?
C14 N1 C17 107.1(2) ?
C2 N1 Cu1 104.17(17) ?
C14 N1 Cu1 112.26(18) ?
C17 N1 Cu1 111.96(17) ?
C15 N4 C3 113.3(2) ?
C15 N4 C5 111.2(2) ?
C3 N4 C5 110.1(2) ?
C15 N4 Cu1 107.17(19) ?
C3 N4 Cu1 102.02(17) ?
C5 N4 Cu1 112.85(19) ?
C9 N8 C7 109.6(2) ?
C9 N8 C24 111.0(3) ?
C7 N8 C24 106.5(2) ?
C9 N8 Cu1 108.14(18) ?
C7 N8 Cu1 112.3(2) ?
C24 N8 Cu1 109.31(18) ?
C10 N11 C12 107.0(2) ?
C10 N11 C16 111.3(2) ?
C12 N11 C16 110.6(2) ?
C10 N11 Cu1 106.24(18) ?
C12 N11 Cu1 114.11(19) ?
C16 N11 Cu1 107.55(18) ?
C32 N31 Cu1 171.3(3) ?
N1 C2 C3 111.2(2) ?
N4 C3 C2 111.7(2) ?
N4 C5 C6 114.8(3) ?
C5 C6 C7 117.4(3) ?
N8 C7 C6 116.8(3) ?
N8 C9 C10 111.2(3) ?
N11 C10 C9 111.6(3) ?
N11 C12 C13 115.2(3) ?
C12 C13 C14 115.8(3) ?
N1 C14 C13 116.9(3) ?
N4 C15 C16 114.4(2) ?
N11 C16 C15 115.1(2) ?
C18 C17 N1 117.0(2) ?
C19 C18 C23 118.2(3) ?
C19 C18 C17 121.7(3) ?
C23 C18 C17 119.9(3) ?
C18 C19 C20 121.0(3) ?
C21 C20 C19 119.8(4) ?
C22 C21 C20 119.9(3) ?
C21 C22 C23 120.7(3) ?
C22 C23 C18 120.5(3) ?
C25 C24 N8 114.5(2) ?
C30 C25 C26 117.9(3) ?
C30 C25 C24 121.0(3) ?
C26 C25 C24 121.1(3) ?
C27 C26 C25 120.5(3) ?
C28 C27 C26 120.5(3) ?
C27 C28 C29 119.7(4) ?
C30 C29 C28 120.1(3) ?
C29 C30 C25 121.3(3) ?
N31 C32 C33 178.2(5) ?
F14 P1 F16 90.9(3) ?
F14 P1 F12 92.7(3) ?
F16 P1 F12 88.65(18) ?
F14 P1 F13 177.8(3) ?
F16 P1 F13 89.3(2) ?
F12 P1 F13 89.4(3) ?
F14 P1 F15 90.5(3) ?
F16 P1 F15 178.4(3) ?
F12 P1 F15 90.66(18) ?
F13 P1 F15 89.3(3) ?
F14 P1 F11 89.5(3) ?
F16 P1 F11 92.07(17) ?
F12 P1 F11 177.7(3) ?
F13 P1 F11 88.4(2) ?
F15 P1 F11 88.57(17) ?
F21 P2 F26 92.8(3) ?
F21 P2 F25 91.7(3) ?
F26 P2 F25 175.1(3) ?
F21 P2 F23 92.98(15) ?
F26 P2 F23 90.9(2) ?
F25 P2 F23 90.7(2) ?
F21 P2 F24 87.86(16) ?
F26 P2 F24 89.5(2) ?
F25 P2 F24 88.87(19) ?
F23 P2 F24 179.09(16) ?
F21 P2 F22 179.2(2) ?
F26 P2 F22 87.7(3) ?
F25 P2 F22 87.8(2) ?
F23 P2 F22 87.57(14) ?
F24 P2 F22 91.60(15) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Cu1 N31 . 2.049(3) y
Cu1 N8 . 2.056(3) y
Cu1 N11 . 2.088(2) y
Cu1 N1 . 2.116(2) y
Cu1 N4 . 2.142(3) y
N1 C2 . 1.497(4) ?
N1 C14 . 1.496(4) ?
N1 C17 . 1.530(4) ?
N4 C15 . 1.485(4) ?
N4 C3 . 1.486(4) ?
N4 C5 . 1.485(4) ?
N8 C9 . 1.499(4) ?
N8 C7 . 1.507(4) ?
N8 C24 . 1.513(4) ?
N11 C10 . 1.495(4) ?
N11 C12 . 1.498(4) ?
N11 C16 . 1.504(4) ?
N31 C32 . 1.182(5) ?
C2 C3 . 1.536(4) ?
C5 C6 . 1.532(5) ?
C6 C7 . 1.533(5) ?
C9 C10 . 1.518(5) ?
C12 C13 . 1.514(4) ?
C13 C14 . 1.523(4) ?
C15 C16 . 1.541(5) ?
C17 C18 . 1.514(4) ?
C18 C19 . 1.394(5) ?
C18 C23 . 1.395(5) ?
C19 C20 . 1.395(5) ?
C20 C21 . 1.380(6) ?
C21 C22 . 1.377(6) ?
C22 C23 . 1.389(5) ?
C24 C25 . 1.507(5) ?
C25 C30 . 1.399(4) ?
C25 C26 . 1.402(5) ?
C26 C27 . 1.388(6) ?
C27 C28 . 1.383(6) ?
C28 C29 . 1.385(5) ?
C29 C30 . 1.383(5) ?
C32 C33 . 1.435(6) ?
P1 F14 . 1.552(4) ?
P1 F16 . 1.562(3) ?
P1 F12 . 1.574(3) ?
P1 F13 . 1.575(4) ?
P1 F15 . 1.584(3) ?
P1 F11 . 1.602(3) ?
P2 F21 . 1.557(3) ?
P2 F26 . 1.559(3) ?
P2 F25 . 1.560(3) ?
P2 F23 . 1.586(2) ?
P2 F24 . 1.589(2) ?
P2 F22 . 1.602(3) ?
