#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/22/4112257.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_4112257
loop_
_publ_author_name
'Shinji Nomura'
'Takahito Itoh'
'Hirofumi Nakasho'
'Takahiro Uno'
'Masataka Kubo'
'Kazuki Sada'
'Katsunari Inoue'
'Mikiji Miyata'
_publ_section_title
;
 Crystal Structures and Topochemical Polymerizations of
 7,7,8,8-Tetrakis(alkoxycarbonyl)quinodimethanes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2035
_journal_page_last               2041
_journal_paper_doi               10.1021/ja0386086
_journal_volume                  126
_journal_year                    2004
_chemical_formula_moiety         'C8 H8 O4 '
_chemical_formula_sum            'C8 H8 O4'
_chemical_formula_weight         168.15
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                96.305(4)
_cell_angle_beta                 105.636(5)
_cell_angle_gamma                87.323(8)
_cell_formula_units_Z            2
_cell_length_a                   8.6023(4)
_cell_length_b                   8.889(2)
_cell_length_c                   5.2870(6)
_cell_measurement_reflns_used    1686
_cell_measurement_temperature    298.2
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      4.0
_cell_volume                     386.90(10)
_computing_cell_refinement       PROCESS
_computing_data_collection       PROCESS
_computing_data_reduction        'teXsan Ver. 1.10'
_computing_publication_material  'teXsan Ver. 1.10'
_computing_structure_refinement  'teXsan Ver. 1.10'
_computing_structure_solution    SIR92
_diffrn_measured_fraction_theta_full 0.9699
_diffrn_measured_fraction_theta_max 0.9699
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       ω
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.033
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            1711
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_exptl_absorpt_coefficient_mu    0.000
_exptl_absorpt_correction_T_max  0.988
_exptl_absorpt_correction_T_min  0.931
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   '(Higashi, 1999)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.443
_exptl_crystal_description       needle
_exptl_crystal_size_max          2.000
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.30
_refine_diff_density_min         -0.33
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.822
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     109
_refine_ls_number_reflns         1711
_refine_ls_R_factor_gt           0.0623
_refine_ls_shift/su_max          0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²) + (0.07300(Max(Fo²,0) + 2Fc²)/3)²]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1834
_reflns_number_gt                1360
_reflns_number_total             1711
_reflns_threshold_expression     F²>2.0σ(F²)
_cod_data_source_file            ja0386086si20030919_041754.cif
_cod_data_source_block           sample2_1a-B
_cod_original_cell_volume        386.87(9)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C8 H8 O4 '
_cod_database_code               4112257
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
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_calc_flag
O(1) O 0.4974(2) -0.3010(2) -0.6416(3) 0.0735(5) Uani 1.00 d
O(2) O 0.7477(2) -0.3944(2) -0.5281(3) 0.0606(4) Uani 1.00 d
O(3) O 0.9557(2) -0.1337(2) -0.2473(3) 0.0709(5) Uani 1.00 d
O(4) O 0.9158(2) -0.2618(2) 0.0643(3) 0.0624(4) Uani 1.00 d
C(1) C 0.5958(2) -0.0982(2) -0.1360(3) 0.0407(4) Uani 1.00 d
C(2) C 0.4220(2) -0.0865(2) -0.2323(3) 0.0445(4) Uani 1.00 d
C(3) C 0.6662(2) -0.0043(2) 0.1042(3) 0.0452(4) Uani 1.00 d
C(4) C 0.6901(2) -0.1916(2) -0.2566(3) 0.0425(4) Uani 1.00 d
C(5) C 0.6297(2) -0.2970(2) -0.4954(3) 0.0466(4) Uani 1.00 d
C(6) C 0.7084(3) -0.5041(3) -0.7538(4) 0.0722(7) Uani 1.00 d
C(7) C 0.8687(2) -0.1923(2) -0.1498(3) 0.0459(4) Uani 1.00 d
C(8) C 1.0842(3) -0.2577(3) 0.2018(5) 0.0795(7) Uani 1.00 d
H(1) H 0.3672 -0.1457 -0.3883 0.0539 Uiso 1.00 calc
H(2) H 0.7797 -0.0068 0.1803 0.0542 Uiso 1.00 calc
H(3) H 0.6800 -0.4532 -0.9109 0.0866 Uiso 1.00 calc
H(4) H 0.6207 -0.5624 -0.7485 0.0866 Uiso 1.00 calc
H(5) H 0.7999 -0.5681 -0.7563 0.0866 Uiso 1.00 calc
H(6) H 1.1467 -0.2907 0.0819 0.0965 Uiso 1.00 calc
H(7) H 1.1054 -0.3223 0.3390 0.0965 Uiso 1.00 calc
H(8) H 1.1121 -0.1569 0.2749 0.0965 Uiso 1.00 calc
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.003 0.002
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
H H 0.000 0.000
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.2)
;
O O 0.011 0.006
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C(5) O(2) C(6) 116.5(2) 1_555 1_555 yes
C(7) O(4) C(8) 117.6(2) 1_555 1_555 yes
C(2) C(1) C(3) 115.4(1) 1_555 1_555 yes
C(2) C(1) C(4) 123.8(1) 1_555 1_555 yes
C(3) C(1) C(4) 120.8(1) 1_555 1_555 yes
C(1) C(2) C(3) 121.8(1) 1_555 2_655 yes
C(1) C(2) H(1) 120.1 1_555 1_555 no
C(3) C(2) H(1) 118.0 2_655 1_555 no
C(1) C(3) C(2) 122.7(1) 1_555 2_655 yes
C(1) C(3) H(2) 120.1 1_555 1_555 no
C(2) C(3) H(2) 117.1 2_655 1_555 no
C(1) C(4) C(5) 125.0(1) 1_555 1_555 yes
C(1) C(4) C(7) 120.3(1) 1_555 1_555 yes
C(5) C(4) C(7) 114.6(1) 1_555 1_555 yes
O(1) C(5) O(2) 122.8(2) 1_555 1_555 yes
O(1) C(5) C(4) 127.6(2) 1_555 1_555 yes
O(2) C(5) C(4) 109.6(1) 1_555 1_555 yes
O(2) C(6) H(3) 109.3 1_555 1_555 no
O(2) C(6) H(4) 110.2 1_555 1_555 no
O(2) C(6) H(5) 109.4 1_555 1_555 no
H(3) C(6) H(4) 109.4 1_555 1_555 no
H(3) C(6) H(5) 108.7 1_555 1_555 no
H(4) C(6) H(5) 109.9 1_555 1_555 no
O(3) C(7) O(4) 124.9(2) 1_555 1_555 yes
O(3) C(7) C(4) 123.0(2) 1_555 1_555 yes
O(4) C(7) C(4) 112.1(1) 1_555 1_555 yes
O(4) C(8) H(6) 109.5 1_555 1_555 no
O(4) C(8) H(7) 109.6 1_555 1_555 no
O(4) C(8) H(8) 109.3 1_555 1_555 no
H(6) C(8) H(7) 109.5 1_555 1_555 no
H(6) C(8) H(8) 109.3 1_555 1_555 no
H(7) C(8) H(8) 109.6 1_555 1_555 no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O(1) C(5) 1.191(2) . yes
O(2) C(5) 1.338(2) . yes
O(2) C(6) 1.431(2) . yes
O(3) C(7) 1.183(2) . yes
O(4) C(7) 1.308(2) . yes
O(4) C(8) 1.435(2) . yes
C(1) C(2) 1.446(2) . yes
C(1) C(3) 1.441(2) . yes
C(1) C(4) 1.362(2) . yes
C(2) C(3) 1.337(3) 2_655 yes
C(2) H(1) 0.947 . no
C(3) H(2) 0.951 . no
C(4) C(5) 1.474(2) . yes
C(4) C(7) 1.487(2) . yes
C(6) H(3) 0.958 . no
C(6) H(4) 0.943 . no
C(6) H(5) 0.952 . no
C(8) H(6) 0.951 . no
C(8) H(7) 0.948 . no
C(8) H(8) 0.951 . no
