An unsymmetrical covalent organic polymer for catalytic amide synthesis.
Yadav, Deepika; Awasthi, Satish Kumar; Dalton transactions (Cambridge, England : 2003) 49 (2020) 179–186; doi:10.1039/c9dt03931g

data_7701999
_publ_section_title
;
 An unsymmetrical covalent organic polymer for catalytic amide synthesis.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              179
_journal_page_last               186
_journal_paper_doi               10.1039/c9dt03931g
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         '0.19(C13 H10 Br N O)'
_chemical_formula_sum            'C2.419 H1.86 Br0.186 N0.186 O0.186'
_chemical_formula_weight         51.37
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_Int_Tables_number      61
_atom_sites_solution_primary     dual
_audit_creation_date             2019-08-22
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.18 svn.r3501 for OlexSys, GUI svn.r5488)
;
_audit_update_record
;
2019-08-22 deposited with the CCDC.	2019-11-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            43
_cell_length_a                   8.1837(8)
_cell_length_b                   9.2427(10)
_cell_length_c                   30.229(3)
_cell_measurement_reflns_used    2494
_cell_measurement_temperature    237(80)
_cell_measurement_theta_max      22.7990
_cell_measurement_theta_min      3.3900
_cell_volume                     2286.5(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      237(80)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9853
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.9926
_diffrn_measured_fraction_theta_max 0.9926
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     -6.00  88.00   1.00    2.50    --   19.00  77.00 150.00   94
  2  \w      4.00  87.00   1.00    2.50    --   19.00  57.00  90.00   83
  3  \w      0.00  85.00   1.00    2.50    --   19.00  57.00   0.00   85
  4  \w     10.00  87.00   1.00    2.50    --   19.00  57.00 -90.00   77
  5  \w    -25.00  59.00   1.00    2.50    --   19.00 -99.00 -60.00   84
  6  \w    -35.00  29.00   1.00    2.50    --  -15.17  38.00-120.00   64
  7  \w    -25.00  59.00   1.00    2.50    --   19.00 -99.00 150.00   84
  8  \w    -45.00  48.00   1.00    2.50    --   19.00 -77.00  30.00   93
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0126106000
_diffrn_orient_matrix_UB_12      0.0343319000
_diffrn_orient_matrix_UB_13      -0.0207042000
_diffrn_orient_matrix_UB_21      -0.0786049000
_diffrn_orient_matrix_UB_22      0.0320349000
_diffrn_orient_matrix_UB_23      0.0014659000
_diffrn_orient_matrix_UB_31      0.0343853000
_diffrn_orient_matrix_UB_32      0.0606363000
_diffrn_orient_matrix_UB_33      0.0109495000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1663
_diffrn_reflns_av_unetI/netI     0.1146
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            31290
_diffrn_reflns_theta_full        24.9993
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.39
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.571
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.44306
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.6042
_exptl_crystal_F_000             1102.2432
_refine_diff_density_max         0.6245
_refine_diff_density_min         -0.6588
_refine_diff_density_rms         0.1692
_refine_ls_d_res_high            0.8409
_refine_ls_d_res_low             6.0050
_refine_ls_goodness_of_fit_ref   0.8854
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    20
_refine_ls_number_parameters     145
_refine_ls_number_reflns         2003
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.8854
_refine_ls_R_factor_all          0.0817
_refine_ls_R_factor_gt           0.0505
_refine_ls_shift/su_max          0.0006
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1324
_refine_ls_wR_factor_ref         0.1584
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              9
_reflns_limit_h_min              0
_reflns_limit_k_max              10
_reflns_limit_k_min              0
_reflns_limit_l_max              35
_reflns_limit_l_min              0
_reflns_number_gt                1393
_reflns_number_total             2003
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c9dt03931g2.cif
_cod_data_source_block           AMZ
_cod_depositor_comments          'Adding full bibliography for 7701999.cif.'
_cod_database_code               7701999
_chemical_oxdiff_formula         'C N H O'
_chemical_oxdiff_usercomment     21-08-2019
_reflns_odcompleteness_completeness 99.56
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C00D(H00D), C00F(H00F), C00E(H00E), C00B(H00B), C009(H009), C00G(H00G),
 C00C(H00C), C00A(H00A), C006(H006), N003(H003)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.641
_oxdiff_exptl_absorpt_empirical_full_min 0.675