Bis(3,4-dimethoxybenzyl) Ether and Tetramethoxy-4,4'-(2,3-dimethyltetramethylene)dipyrocatechol
Hoong-Kun Fun; Kandasamy Chinnakali; Kandasamy Sivakumar; Teng-Wah Sam; Siew-Eng How; Acta Crystallographica Section C 53 (1997) 1857–1859; doi:10.1107/S0108270197009761

data_2006857
_publ_section_title
;
 Bis(3,4-dimethoxybenzyl) Ether and
 Tetramethoxy-4,4'-(2,3-dimethyltetramethylene)dipyrocatechol
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1857
_journal_page_last               1859
_journal_paper_doi               10.1107/S0108270197009761
_journal_volume                  53
_journal_year                    1997
_chemical_formula_sum            'C18 H22 O5'
_chemical_formula_weight         318.36
_chemical_melting_point          74.9(5)
_chemical_name_systematic
;
Bis(3,4-dimethoxybenzyl)ether
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 93.020(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.3990(10)
_cell_length_b                   5.8060(10)
_cell_length_c                   28.126(2)
_cell_measurement_reflns_used    52
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.34
_cell_measurement_theta_min      2.77
_cell_volume                     1695.8(4)
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4 diffractometer'
_diffrn_measurement_method       '\q/2\q scans'
_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  0.0338
_diffrn_reflns_av_sigmaI/netI    0.0546
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            5423
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.45
_diffrn_standards_decay_%        <3
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.090
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.247
_exptl_crystal_density_meas      ?
_exptl_crystal_description       rectangular
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.68
_exptl_crystal_size_mid          0.62
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.14
_refine_diff_density_min         -0.12
_refine_ls_extinction_coef       0.0216(15)
_refine_ls_extinction_method     'SHELXL93 (Sheldrick, 1993)'
_refine_ls_goodness_of_fit_all   0.865
_refine_ls_goodness_of_fit_obs   1.044
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     297
_refine_ls_number_reflns         3911
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.865
_refine_ls_restrained_S_obs      1.044
_refine_ls_R_factor_all          0.0842
_refine_ls_R_factor_obs          .0398
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0553P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1104
_refine_ls_wR_factor_obs         .0960
_reflns_number_observed          2158
_reflns_number_total             3911
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            mu1334.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '74.4-75.4' was changed to '74.9(5)'
- the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_chemical_melting_point' value '74.4-75.4' was changed to '74.9(5)'
- the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0553P)^2^] where P=(Fo^2^+2Fc^2^)/3' was changed
to 'calc'. New tag '_refine_ls_weighting_details' was created. The
value of the new tag was set to 'w = 1/[\s^2^(Fo^2^)+(0.0553P)^2^]
where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1695.8(2)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2006857