#------------------------------------------------------------------------------
#$Date: 2019-11-05 19:18:30 +0100 (mar 05 de nov de 2019) $
#$Revision: 223360 $
#$URL: svn://www.crystallography.net/cod/cif/7/70/17/7701798.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_7701798
loop_
_publ_author_name
'Hu, Min-Na'
'Zhang, Wen-Qian'
'Liu, Hua'
'He, Peng-Xiu'
'Liu, Ping'
'Wang, Yao-Yu'
'Li, Jian-Li'
_publ_section_title
;
 Five complexes based on a new racemic tetraoxaspiro ligand: correlation
 of potential coordination preferences with the structure, magnetic
 properties and luminescence properties.
;
_journal_issue                   12
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3862
_journal_page_last               3873
_journal_paper_doi               10.1039/c8dt04051f
_journal_volume                  48
_journal_year                    2019
_chemical_formula_sum            'C17 H18 N2 O4'
_chemical_formula_weight         314.33
_space_group_crystal_system      orthorhombic
_space_group_IT_number           41
_space_group_name_Hall           'A 2 -2ab'
_space_group_name_H-M_alt        'A e a 2'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/ccdc.csd.cc205msm
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-12-25 deposited with the CCDC.
2019-01-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.479(7)
_cell_length_b                   10.978(3)
_cell_length_c                   5.6901(16)
_cell_measurement_reflns_used    1230
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      23.28
_cell_measurement_theta_min      3.33
_cell_volume                     1529.1(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0301
_diffrn_reflns_av_unetI/netI     0.0425
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            4516
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.227
_diffrn_reflns_theta_min         1.664
_exptl_absorpt_coefficient_mu    0.098
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.365
_exptl_crystal_description       block
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.170
_refine_diff_density_max         0.240
_refine_diff_density_min         -0.230
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details
;
 Flack x determined using 499 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   1.3(8)
_refine_ls_extinction_coef       0.011(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     106
_refine_ls_number_reflns         1810
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0593
_refine_ls_R_factor_gt           0.0421
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0458P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0865
_refine_ls_wR_factor_ref         0.0938
_reflns_Friedel_coverage         0.750
_reflns_Friedel_fraction_full    0.979
_reflns_Friedel_fraction_max     0.908
_reflns_number_gt                1411
_reflns_number_total             1810
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8dt04051f2.cif
_cod_data_source_block           1_CCDC3
_cod_original_sg_symbol_Hall     'A 2 -2ac'
_cod_original_sg_symbol_H-M      'A b a 2'
_cod_database_code               7701798
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.981
_shelx_estimated_absorpt_t_max   0.983
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'x+1/2, -y+1, z+1/2'
'-x+1/2, y+1, 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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
C1 C 0.70023(10) 0.6359(2) 0.0478(5) 0.0524(7) Uani 1 1 d . . .
H1 H 0.7223 0.5804 -0.0314 0.063 Uiso 1 1 calc R U .
C2 C 0.69512(11) 0.7512(2) -0.0435(5) 0.0553(7) Uani 1 1 d . . .
H2 H 0.7138 0.7729 -0.1797 0.066 Uiso 1 1 calc R U .
C3 C 0.66206(10) 0.8341(2) 0.0691(5) 0.0485(7) Uani 1 1 d . . .
H3 H 0.6578 0.9124 0.0095 0.058 Uiso 1 1 calc R U .
C4 C 0.63521(8) 0.79903(19) 0.2729(4) 0.0364(5) Uani 1 1 d . . .
C5 C 0.64367(10) 0.6809(2) 0.3522(5) 0.0422(6) Uani 1 1 d . . .
H5 H 0.6262 0.6569 0.4897 0.051 Uiso 1 1 calc R U .
C6 C 0.59959(9) 0.88688(19) 0.4072(4) 0.0378(5) Uani 1 1 d . . .
H6 H 0.6221 0.9325 0.5193 0.045 Uiso 1 1 calc R U .
C7 C 0.54395(10) 1.0589(2) 0.3651(4) 0.0423(6) Uani 1 1 d . . .
H7A H 0.5268 1.1121 0.2508 0.051 Uiso 1 1 calc R U .
H7B H 0.5677 1.1081 0.4629 0.051 Uiso 1 1 calc R U .
C8 C 0.5000 1.0000 0.5180(5) 0.0365(7) Uani 1 2 d S T P
C9 C 0.52720(10) 0.9034(2) 0.6711(4) 0.0450(6) Uani 1 1 d . . .
H9A H 0.5506 0.9427 0.7861 0.054 Uiso 1 1 calc R U .
H9B H 0.4994 0.8579 0.7551 0.054 Uiso 1 1 calc R U .
N1 N 0.67544(8) 0.59956(18) 0.2429(4) 0.0500(6) Uani 1 1 d . . .
O1 O 0.57594(6) 0.96843(13) 0.2445(3) 0.0421(4) Uani 1 1 d . . .
O2 O 0.55915(6) 0.82152(13) 0.5299(3) 0.0423(4) Uani 1 1 d . . .
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'
N N 0.0061 0.0033 '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'
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
N1 C1 C2 123.5(3) . .
N1 C1 H1 118.2 . .
C2 C1 H1 118.2 . .
C1 C2 C3 119.1(3) . .
C1 C2 H2 120.4 . .
C3 C2 H2 120.4 . .
C2 C3 C4 119.0(2) . .
C2 C3 H3 120.5 . .
C4 C3 H3 120.5 . .
C3 C4 C5 117.4(2) . .
C3 C4 C6 121.4(2) . .
C5 C4 C6 121.2(2) . .
N1 C5 C4 124.0(2) . .
N1 C5 H5 118.0 . .
C4 C5 H5 118.0 . .
O2 C6 O1 111.10(17) . .
O2 C6 C4 109.39(17) . .
O1 C6 C4 108.05(19) . .
O2 C6 H6 109.4 . .
O1 C6 H6 109.4 . .
C4 C6 H6 109.4 . .
O1 C7 C8 111.29(15) . .
O1 C7 H7A 109.4 . .
C8 C7 H7A 109.4 . .
O1 C7 H7B 109.4 . .
C8 C7 H7B 109.4 . .
H7A C7 H7B 108.0 . .
C9 C8 C9 110.3(2) 2_675 .
C9 C8 C7 108.20(13) 2_675 2_675
C9 C8 C7 109.81(14) . 2_675
C9 C8 C7 109.81(14) 2_675 .
C9 C8 C7 108.19(13) . .
C7 C8 C7 110.5(2) 2_675 .
O2 C9 C8 110.67(17) . .
O2 C9 H9A 109.5 . .
C8 C9 H9A 109.5 . .
O2 C9 H9B 109.5 . .
C8 C9 H9B 109.5 . .
H9A C9 H9B 108.1 . .
C1 N1 C5 117.0(2) . .
C6 O1 C7 110.36(17) . .
C6 O2 C9 109.94(16) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.327(3) .
C1 C2 1.373(4) .
C1 H1 0.9300 .
C2 C3 1.376(4) .
C2 H2 0.9300 .
C3 C4 1.387(3) .
C3 H3 0.9300 .
C4 C5 1.389(3) .
C4 C6 1.508(3) .
C5 N1 1.338(3) .
C5 H5 0.9300 .
C6 O2 1.408(3) .
C6 O1 1.412(2) .
C6 H6 0.9800 .
C7 O1 1.439(3) .
C7 C8 1.527(3) .
C7 H7A 0.9700 .
C7 H7B 0.9700 .
C8 C9 1.525(3) 2_675
C8 C9 1.525(3) .
C8 C7 1.527(3) 2_675
C9 O2 1.438(3) .
C9 H9A 0.9700 .
C9 H9B 0.9700 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
N1 C1 C2 C3 -1.0(4) . .
C1 C2 C3 C4 0.5(4) . .
C2 C3 C4 C5 0.3(3) . .
C2 C3 C4 C6 178.4(2) . .
C3 C4 C5 N1 -0.8(3) . .
C6 C4 C5 N1 -178.9(2) . .
C3 C4 C6 O2 152.8(2) . .
C5 C4 C6 O2 -29.2(3) . .
C3 C4 C6 O1 31.7(3) . .
C5 C4 C6 O1 -150.23(19) . .
O1 C7 C8 C9 171.36(18) . 2_675
O1 C7 C8 C9 50.9(2) . .
O1 C7 C8 C7 -69.35(15) . 2_675
C9 C8 C9 O2 -172.1(2) 2_675 .
C7 C8 C9 O2 68.7(2) 2_675 .
C7 C8 C9 O2 -52.0(2) . .
C2 C1 N1 C5 0.5(4) . .
C4 C5 N1 C1 0.4(3) . .
O2 C6 O1 C7 63.3(2) . .
C4 C6 O1 C7 -176.68(17) . .
C8 C7 O1 C6 -56.7(2) . .
O1 C6 O2 C9 -64.6(2) . .
C4 C6 O2 C9 176.17(18) . .
C8 C9 O2 C6 59.2(2) . .
