#------------------------------------------------------------------------------
#$Date: 2016-03-21 06:05:04 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178489 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/00/4060072.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4060072
loop_
_publ_author_name
'Jens Langer'
'Helmar Görls'
'Reinald Fischer'
'Dirk Walther'
_publ_section_title
;
 Organometallic Nickelamacrocycles of the Type [(R2R'P)Ni(C2H4COO)]n:
 Synthesis and Self-Assembly to Form Different Molecular Architectures
 Tuned by the Phosphine
;
_journal_name_full               Organometallics
_journal_page_first              272
_journal_page_last               279
_journal_paper_doi               10.1021/om040111x
_journal_volume                  24
_journal_year                    2005
_chemical_formula_sum            'C84 H148 Ni4 O8 P4'
_chemical_formula_weight         1644.74
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           82
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I -4'
_symmetry_space_group_name_H-M   'I -4'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   18.7303(4)
_cell_length_b                   18.7303(4)
_cell_length_c                   12.5854(2)
_cell_measurement_temperature    183(2)
_cell_volume                     4415.26(15)
_computing_cell_refinement       DENZO
_computing_data_collection       COLLECT
_computing_data_reduction        DENZO
_computing_molecular_graphics    SHELXTL/PC
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      183(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'phi- + omega-scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0442
_diffrn_reflns_av_sigmaI/netI    0.0460
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            15825
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.92
_exptl_absorpt_coefficient_mu    0.962
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.237
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1776
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.772
_refine_diff_density_min         -0.348
_refine_diff_density_rms         0.130
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.486(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         5043
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0594
_refine_ls_R_factor_gt           0.0482
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1034P)²+0.5167P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1358
_refine_ls_wR_factor_ref         0.1441
_reflns_number_gt                4408
_reflns_number_total             5043
_reflns_threshold_expression     >2sigma(I)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'NONE' changed to 'none' according
to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

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

The following automatic conversions were performed:

'_symmetry_cell_setting' tag value 'tetragonalic' was replaced with
'tetragonal' value.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_sg_symbol_H-M      I-4
_cod_database_code               4060072
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Ni Ni 0.59797(2) 0.39367(2) 0.10546(3) 0.02323(14) Uani 1 1 d .
P1 P 0.59397(5) 0.29678(5) 0.19618(8) 0.0246(2) Uani 1 1 d .
O1 O 0.61305(15) 0.47908(14) 0.0269(2) 0.0277(6) Uani 1 1 d .
O2 O 0.65340(15) 0.59001(15) 0.0356(2) 0.0291(6) Uani 1 1 d .
C1 C 0.6065(2) 0.4549(2) 0.2284(3) 0.0288(8) Uani 1 1 d .
H1A H 0.5590 0.4726 0.2508 0.035 Uiso 1 1 calc R
H1B H 0.6284 0.4287 0.2885 0.035 Uiso 1 1 calc R
C2 C 0.6544(2) 0.5170(2) 0.1935(3) 0.0286(8) Uani 1 1 d .
H2A H 0.6439 0.5600 0.2364 0.034 Uiso 1 1 calc R
H2B H 0.7053 0.5043 0.2036 0.034 Uiso 1 1 calc R
C3 C 0.6395(2) 0.5313(2) 0.0777(3) 0.0245(7) Uani 1 1 d .
C4 C 0.5515(2) 0.3000(2) 0.3284(3) 0.0315(9) Uani 1 1 d .
H4A H 0.5836 0.3305 0.3728 0.038 Uiso 1 1 calc R
C5 C 0.4789(2) 0.3386(3) 0.3281(4) 0.0393(10) Uani 1 1 d .
H5A H 0.4838 0.3856 0.2929 0.047 Uiso 1 1 calc R
H5B H 0.4437 0.3101 0.2876 0.047 Uiso 1 1 calc R
C6 C 0.4527(3) 0.3489(3) 0.4420(4) 0.0500(13) Uani 1 1 d .
H6A H 0.4863 0.3804 0.4805 0.060 Uiso 1 1 calc R
H6B H 0.4055 0.3726 0.4409 0.060 Uiso 1 1 calc R
C7 C 0.4467(3) 0.2791(4) 0.4994(5) 0.0611(16) Uani 1 1 d .
H7A H 0.4104 0.2489 0.4640 0.073 Uiso 1 1 calc R
H7B H 0.4308 0.2878 0.5733 0.073 Uiso 1 1 calc R
C8 C 0.5179(3) 0.2401(4) 0.5007(4) 0.0564(14) Uani 1 1 d .
H8A H 0.5120 0.1933 0.5362 0.068 Uiso 1 1 calc R
H8B H 0.5530 0.2683 0.5420 0.068 Uiso 1 1 calc R
C9 C 0.5462(3) 0.2286(2) 0.3879(4) 0.0383(10) Uani 1 1 d .
H9A H 0.5139 0.1960 0.3489 0.046 Uiso 1 1 calc R
H9B H 0.5940 0.2060 0.3912 0.046 Uiso 1 1 calc R
C10 C 0.6859(2) 0.2647(2) 0.2224(3) 0.0288(8) Uani 1 1 d .
H10A H 0.6831 0.2156 0.2535 0.035 Uiso 1 1 calc R
C11 C 0.7261(2) 0.3130(3) 0.2999(3) 0.0352(9) Uani 1 1 d .
H11A H 0.7021 0.3117 0.3700 0.042 Uiso 1 1 calc R
H11B H 0.7245 0.3628 0.2736 0.042 Uiso 1 1 calc R
C12 C 0.8044(2) 0.2899(3) 0.3132(4) 0.0395(10) Uani 1 1 d .
H12A H 0.8289 0.3232 0.3622 0.047 Uiso 1 1 calc R
H12B H 0.8062 0.2416 0.3449 0.047 Uiso 1 1 calc R
C13 C 0.8422(2) 0.2895(3) 0.2079(4) 0.0411(11) Uani 1 1 d .
H13A H 0.8921 0.2731 0.2177 0.049 Uiso 1 1 calc R
H13B H 0.8433 0.3384 0.1782 0.049 Uiso 1 1 calc R
C14 C 0.8024(3) 0.2383(3) 0.1295(4) 0.0458(12) Uani 1 1 d .
H14A H 0.8268 0.2389 0.0597 0.055 Uiso 1 1 calc R
H14B H 0.8042 0.1889 0.1574 0.055 Uiso 1 1 calc R
C15 C 0.7260(2) 0.2606(2) 0.1157(4) 0.0352(9) Uani 1 1 d .
H15A H 0.7016 0.2260 0.0687 0.042 Uiso 1 1 calc R
H15B H 0.7245 0.3079 0.0808 0.042 Uiso 1 1 calc R
C16 C 0.5539(2) 0.2233(2) 0.1173(3) 0.0319(9) Uani 1 1 d .
H16A H 0.5719 0.2308 0.0433 0.038 Uiso 1 1 calc R
C17 C 0.5737(3) 0.1452(2) 0.1444(4) 0.0406(10) Uani 1 1 d .
H17A H 0.6262 0.1402 0.1488 0.049 Uiso 1 1 calc R
H17B H 0.5531 0.1320 0.2141 0.049 Uiso 1 1 calc R
C18 C 0.5446(3) 0.0958(3) 0.0585(4) 0.0503(13) Uani 1 1 d .
H18A H 0.5559 0.0457 0.0773 0.060 Uiso 1 1 calc R
H18B H 0.5684 0.1068 -0.0098 0.060 Uiso 1 1 calc R
C19 C 0.4641(3) 0.1036(3) 0.0449(4) 0.0497(13) Uani 1 1 d .
H19A H 0.4399 0.0870 0.1103 0.060 Uiso 1 1 calc R
H19B H 0.4481 0.0730 -0.0146 0.060 Uiso 1 1 calc R
C20 C 0.4427(3) 0.1809(3) 0.0227(4) 0.0498(13) Uani 1 1 d .
H20A H 0.4618 0.1957 -0.0473 0.060 Uiso 1 1 calc R
H20B H 0.3900 0.1846 0.0200 0.060 Uiso 1 1 calc R
C21 C 0.4714(2) 0.2309(2) 0.1086(4) 0.0359(9) Uani 1 1 d .
H21A H 0.4491 0.2191 0.1777 0.043 Uiso 1 1 calc R
H21B H 0.4589 0.2809 0.0908 0.043 Uiso 1 1 calc R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 '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_site_symmetry_1
_geom_angle_site_symmetry_3
O1 Ni C1 84.57(15) . .
O1 Ni O2 85.40(12) . 3_565
C1 Ni O2 169.91(15) . 3_565
O1 Ni P1 173.44(9) . .
C1 Ni P1 94.50(12) . .
O2 Ni P1 95.59(9) 3_565 .
C4 P1 C10 104.49(19) . .
C4 P1 C16 109.42(19) . .
C10 P1 C16 103.33(19) . .
C4 P1 Ni 117.86(14) . .
C10 P1 Ni 109.69(14) . .
C16 P1 Ni 110.89(14) . .
C3 O1 Ni 116.4(2) . .
C3 O2 Ni 110.7(2) . 4_655
C2 C1 Ni 105.6(3) . .
C3 C2 C1 107.7(3) . .
O2 C3 O1 123.1(3) . .
O2 C3 C2 121.9(3) . .
O1 C3 C2 114.9(3) . .
C9 C4 C5 110.7(4) . .
C9 C4 P1 116.1(3) . .
C5 C4 P1 113.2(3) . .
C6 C5 C4 109.9(4) . .
C7 C6 C5 111.5(5) . .
C6 C7 C8 111.0(4) . .
C7 C8 C9 111.2(5) . .
C8 C9 C4 110.6(4) . .
C11 C10 C15 110.2(3) . .
C11 C10 P1 112.3(3) . .
C15 C10 P1 108.3(3) . .
C10 C11 C12 111.9(4) . .
C13 C12 C11 110.8(4) . .
C12 C13 C14 109.5(4) . .
C15 C14 C13 110.9(4) . .
C14 C15 C10 112.2(4) . .
C17 C16 C21 109.9(3) . .
C17 C16 P1 119.1(3) . .
C21 C16 P1 111.8(3) . .
C18 C17 C16 109.4(4) . .
C17 C18 C19 112.0(4) . .
C18 C19 C20 111.8(4) . .
C21 C20 C19 111.1(4) . .
C20 C21 C16 110.0(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni O1 1.902(3) .
Ni C1 1.933(4) .
Ni O2 1.987(3) 3_565
Ni P1 2.1454(11) .
P1 C4 1.845(4) .
P1 C10 1.853(4) .
P1 C16 1.856(4) .
O1 C3 1.270(5) .
O2 C3 1.248(5) .
O2 Ni 1.987(3) 4_655
C1 C2 1.533(6) .
C2 C3 1.509(5) .
C4 C9 1.536(6) .
C4 C5 1.540(6) .
C5 C6 1.527(7) .
C6 C7 1.499(9) .
C7 C8 1.521(9) .
C8 C9 1.530(7) .
C10 C11 1.528(6) .
C10 C15 1.541(6) .
C11 C12 1.538(6) .
C12 C13 1.503(7) .
C13 C14 1.565(7) .
C14 C15 1.501(6) .
C16 C17 1.548(6) .
C16 C21 1.556(6) .
C17 C18 1.523(7) .
C18 C19 1.523(8) .
C19 C20 1.529(8) .
C20 C21 1.527(6) .
