A robust and modular synthesis of ynamides
Steven J. Mansfield; Craig D. Campbell; Michael W. Jones; Edward A. Anderson; Chem.Commun. 51 (2015) 3316–; doi:10.1039/C4cc07876D

data_7116514
_publ_section_title
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 A robust and modular synthesis of ynamides
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_journal_name_full               Chem.Commun.
_journal_page_first              3316
_journal_paper_doi               10.1039/C4cc07876D
_journal_volume                  51
_journal_year                    2015
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C5 H5 Cl2 N O2'
_chemical_formula_sum            'C5 H5 Cl2 N O2'
_chemical_formula_weight         182.01
_chemical_melting_point          ?
_chemical_name_systematic        010mwj14
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P -2n 2a'
_symmetry_space_group_name_H-M   'P 21 c n'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_creation_date             2014-08-02
_audit_creation_method           CRYSTALS_ver_14.43
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.8679(2)
_cell_length_b                   10.4250(3)
_cell_length_c                   11.8622(3)
_cell_measurement_reflns_used    1003
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     725.64(4)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_pressure         102
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.018
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9210
_diffrn_reflns_theta_full        27.465
_diffrn_reflns_theta_max         27.465
_diffrn_reflns_theta_min         5.207
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.828
_exptl_absorpt_correction_T_max  0.94
_exptl_absorpt_correction_T_min  0.91
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.666
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             368
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.30
_refine_diff_density_min         -0.33
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9883
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     128
_refine_ls_number_reflns         909
_refine_ls_number_restraints     57
_refine_ls_R_factor_all          0.0363
_refine_ls_R_factor_gt           0.0305
_refine_ls_shift/su_max          0.0055448
_refine_ls_shift/su_mean         0.0004432
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
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 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 5.22 6.36 1.86 
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_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0622
_refine_ls_wR_factor_gt          0.0563
_refine_ls_wR_factor_ref         0.0622
_reflns_limit_h_max              7
_reflns_limit_h_min              0
_reflns_limit_k_max              13
_reflns_limit_k_min              0
_reflns_limit_l_max              15
_reflns_limit_l_min              0
_reflns_number_gt                814
_reflns_number_total             909
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.51
_oxford_diffrn_Wilson_scale      3.78
_oxford_refine_ls_r_factor_ref   0.0363
_oxford_refine_ls_scale          0.4992(9)
_oxford_reflns_number_all        909
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title '010mwj14 At 10:15 on 31/ 7'
_iucr_refine_instructions_details_constraints
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BLOCK SCALE X'S, U'S 
EQUIV PART(0003,OCC) PART(0004,OCC) 
WEIGHT -1 PART(0004,OCC) 
END                                                                             
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_iucr_refine_instructions_details_restraints
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NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
DISTANCE 1.450000 , 0.050000 = C(70) TO N(30) 
DISTANCE 1.450000 , 0.050000 = C(21) TO N(30) 
DISTANCE 1.450000 , 0.050000 = C(2) TO N(31) 
U(IJ)'S  0.0, 0.010000 = N(30) TO N(31) 
U(IJ)'S  0.0, 0.010000 = C(2) TO C(21) 
U(IJ)'S  0.0, 0.010000 = C(9) TO C(22) 
U(IJ)'S  0.0, 0.010000 = C(70) TO C(71) 
DISTANCE 1.450000 , 0.050000 = C(4) TO N(30) 
VIBRATION 0.0, 0.010000 = N(30) TO N(31) 
VIBRATION 0.0, 0.010000 = C(70) TO C(71) 
VIBRATION 0.0, 0.010000 = C(2) TO C(21) 
VIBRATION 0.0, 0.010000 = C(9) TO C(22) 
SAME 0.01, 0.1 FOR C(71) N(31) C(4) C(2)  C(9)  CL(1) AND 
CONT               C(70) N(30) C(4) C(21) C(22) CL(10) 
VIBRATION 0.0, 0.010000 = C(6) TO C(70) 
VIBRATION 0.0, 0.010000 = C(70) TO N(30) 
END                                                                             
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_cod_data_source_file            c4cc07876d2.cif
_cod_data_source_block           2t
_cod_depositor_comments
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The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

'_atom_sites_solution_primary'
value 'Other' changed to 'other' according to the built-in table from
CIF Core dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

Automatic conversion script
Id: cif_fix_values 2827 2014-09-09 07:05:25Z andrius 
;
_cod_original_sg_symbol_Hall     'P -2n 2a '
_cod_original_sg_symbol_H-M      'P 21 c n '
_cod_database_code               7116514